Residual Solvent Analysis

Complete Solutions for Residual Solvent Testing

• How to successfully implement

the USP <467> revision.
• Improve system suitability pass
rates with an optimized system.
• Save column evaluation time and
expense using a retention time index.

Chromatography Products
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The Chemistry of Static Headspace Gas Chromatography
Improve Method Performance with Fundamentals
Figure 1 Volatile components partition into Organic volatile impurities (OVIs), commonly referred to as residual solvents,
gaseous phase until equilibrium is reached. are trace level chemical residues in drug substances and drug products that are
byproducts of manufacturing or that form during packaging and storage. Drug
Final manufacturers must ensure that these residues are removed, or are present only
Gaseous Phase
Concentration in limited concentrations. The International Conference on Harmonization
(ICH) Q3C guideline lists the acceptable amounts of solvent residues that can
CG be present. Methodology, both independently developed and compendial,
VG Gaseous Phase should strive to coincide with this guideline. In this guide, we will take a com-
"Headspace"
Δ Temp. prehensive look at residual solvent analysis, in both theory and practice, and
VV Δ Time illustrate options for the practicing chromatographer.
Sample CO The analysis of residual solvents is commonly performed using static headspace
VS
phase gas chromatography (HS/GC). The basic premise behind headspace analysis
Initial
Sample Phase begins with the addition of an exact, known volume or weight of sample into a
Concentration closed, sealed vial. This creates two distinct phases in the vial—a sample phase
and a gaseous phase, or “headspace”. Volatile components inside the sample
Solvent Molecule Volatile Analyte Molecule
phase, whether a solid or solution, can be extracted, or partitioned, from the
Once the sample phase is introduced into the vial and the vial is sample phase into the headspace. An aliquot of the headspace can then be taken
sealed, volatile components diffuse into the gas phase until the and delivered into a GC system for separation and detection. If we look at the
headspace has reached a state of equilibrium as depicted by the
arrows. The sample is then taken from the headspace.
anatomy of a headspace vial (Figure 1), we can begin to see the relationship of
the vial components and how we can control these parameters to create analyt-
ical methods.
Figure 2 Fundamental headspace relationship.
Residual solvent analysis by static HS/GC can be enhanced by careful consider-
ation of two basic concepts—partition coefficient (K) and phase ratio (β).
CO
A α CG = Phase Ratio Partition coefficients and phase ratios work together to determine the final con-
K+β β= VG / VS centration of volatile compounds in the headspace of sample vials. Volatile com-
Volume dependent ponents partition from the sample phase and equilibrate in the vial headspace.
Striving for the lowest values for both K and β when preparing samples will
Partition Coefficient 1
K= CS / CG Kα result in higher concentrations of volatile analytes in the gas phase and, there-
Pi0 - γi fore, better sensitivity (Figure 2).
Concentration
dependent
Vapor Pressure (Pi0) Activity Coefficient (γi) Controlling the Partition Coefficient
Affected by Temperature Affected by salting-out
Where: Affected by foreign solvent The partition coefficient (K) is defined as the equilibrium distribution of an
A = area Affected by derivitization
VG = volume of gas phase
analyte between the sample and gas phases. Compounds that have low K values
VS = volume of sample phase will tend to partition more readily into the gas phase, and have relatively high
VV = total vial volume
CO = initial analyte concentration in sample responses and low limits of detection. K can be further described as a relation-
CG = analyte concentration in gas phase ship between analyte vapor pressure (pi0) and activity coefficient (γi). In prac-
CS = analyte concentration in sample phase
Pi0 = analyte vapor pressure tice, K can be lowered by increasing the temperature at which the vial is equili-
γi = activity coefficient brated (vapor pressure) or by changing the composition of the sample matrix
(activity coefficient) by adding an inorganic salt or a solvent of lesser solubility,
often referred to as a foreign solvent. High salt concentrations and foreign sol-
Technical Opportunities vents decrease analyte solubility in the sample phase (decrease activity) and pro-
Expand your knowledge and improve your mote transfer into the headspace, thus resulting in lower K values. The magni-
results with Restek. tude of this effect on K is not the same for all analytes. Compounds with inher-
ent low K values in the matrix will experience little change in partition coeffi-
• Request our free Technical Guide for Static
cient in response to the addition of a salt and temperature, while volatile com-
Headspace Analysis. cat.# 59895A
pounds in a matrix of similar polarity will show the largest responses.
• Review our technical poster on dual column
analysis of residual solvents. Adjusting the Phase Ratio
The phase ratio (β) is defined as the volume of the headspace over the volume
of the sample in the vial. Lower values for β (i.e., larger sample sizes) will yield
higher responses for compounds with inherently low K values. However,
decreasing β will not always yield the increase in response needed to improve
sensitivity. When β is decreased by increasing sample size, compounds with high
www.restek.com/ovi K values will partition less into the headspace compared to compounds with low
K values and yield correspondingly smaller changes in sensitivity.

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 Achieving USP<467> Compliance
Your Guide to Successfully Implementing the Revised Method
The USP general chapter <467> Residual Solvents is a widely used compendial
method for identifying and quantifying residual solvents when no information
is available on what solvents are likely to be present. In an attempt to harmonize Restek carries a full
with the ICH guidelines, the USP has proposed a more comprehensive method
in the current USP 30/NF 25. This revision significantly increases the number of
line of headspace
residual solvents to be routinely tested and includes three distinct procedures.1 essentials
Initially set to become effective July 1, 2007, the implementation of the current including screw-thread headspace vials
version of USP <467> has been delayed until July 1, 2008. Until that time, the & magnetic screw-thread caps!
Other Analytical Procedures section of the previous version will be retained.
However, in preparation for the implementation of the revised method, this
application will comply with the procedure and criteria set forth in the USP30/
NF25, second supplement (effective December 1, 2007) and the interim revision
announcement.
Overview of Method
The revised USP <467> method consists of a static headspace extraction cou-
pled with a gas chromatographic separation and flame ionization detection. In
this guide we demonstrate the USP <467> application using two different types
of headspace autosamplers. Procedure A was performed using a pressured loop
autosampler and transfer line. Procedure B was performed using a heated
syringe injection. Either system can be used to meet method requirements.
USP <467> is divided into two separate sections based upon sample solubility:
water-soluble and water-insoluble articles. The methodology for both types of Visit www.restek.com
articles is similar, but the diluent used in both standard and sample preparations
differs based upon the solubility of the test article. The test method consists of
for a complete selection.
three procedures (A, B, and C), that are designed to identify, confirm, and then
quantify residual solvents in drug substances and products (Figure 3).

Figure 3 Analytical flow chart for residual solvent testing under the tech tip
revised USP <467> method. Compatibility concerns?
Procedure A Procedure B Procedure C Refer to the Septum Selection Guide
Identification Confirmation Quantification at www.restek.com/septaguide

Prepare Standard Prepare Standard

and Test Solutions and Test Solutions

Perform Procedure Under

Method-Specified System
Perform Procedure Under
Method-Specified System free literature
and Conditions and Conditions
Download your free copy of
YES YES our Technical Guide for Static
Residual Solvents Residual Solvents Headspace Analysis from
Peaks Present at an Peaks Present at an www.restek.com/ovi
Area Greater than the Area Greater than the
Corresponding Corresponding lit. cat.# 59895A
Standard? Standard?

NO NO

Passes Test Passes Test Calculate Amount of

No Further Action No Further Action Residual Solvents Present

1
This number of analytes to be tested represents the sum of Class 1 and 2 residual solvents that
can be effectively assayed using HS/GC. The actual number of analytes may be more if xylenes,
ethyl benzene and cis/trans 1,2 dichloroethylene are differentiated, or if circumstances require
the quantification of specific Class 3 residual solvents.

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Achieving USP<467> Compliance (continued from page 3)

Analytical Reference Materials

USP-equivalent standards The ICH guideline classifies residual solvents by class according to toxicity. Class
Visit us online at www.restek.com 1 compounds are carcinogenic and pose a risk to both the consumer and the
environment. The use of these solvents must be avoided or tightly controlled.
Class 2 compounds are nongenotoxic animal carcinogens and their concentra-
tion should be limited. Both Class 1 and 2 compounds require chromatograph-
ic determination and are separated into 3 test mixes: Class 1 Mixture, Class 2
Mixture A, and Class 2 Mixture B. Class 3 compounds have low toxic potential.
Concentration levels of up to 0.5% are acceptable and, therefore, they can be
assayed by nonspecific techniques, such as weight loss on drying. Class 2
Mixture C is not used in the second supplement of USP 30/NF 25, but contains
solvents that are not readily detectable by headspace analysis. These solvents
should be assayed by other appropriately validated procedures.
Procedure A - Identification
Residual Solvents - Class 1 Procedure A is the first step in the identification process and is performed on a
benzene 10mg/mL 1,1-dichloroethene 40 G43 column to determine if any residual solvents are present in the sample at
carbon tetrachloride 20 1,1,1-trichloroethane 50 detectable levels. First, Class 1 standard and system suitability solutions and
1,2-dichloroethane 25
Class 2 Mix A standard solutions are assayed under the method-specified oper-
In dimethyl sulfoxide, 1mL/ampul
ating conditions to establish system suitability. All peaks in the Class 1 system
cat. # 36279 (ea.)
suitability solution must have a signal-to-noise ratio not less than 3, the Class 1
Quantity discounts not available.
standard solution must have a 1,1,1-trichloroethane response greater than 5,
and the resolution of acetonitrile and dichloromethane must be not less than 1
Residual Solvents Class 2 - Mix A (15 components) in the Class 2 Mixture A solution. When system suitability has been achieved, the
acetonitrile 2.05mg/mL methylcyclohexane 5.90 test solutions are assayed along with the Class 1 and Class 2 Mixtures A and B
chlorobenzene 1.80 methylene chloride 3.00
cyclohexane 19.40 tetrahydrofuran 3.45 standard solutions. If a peak is determined in the sample that matches a reten-
cis-1,2-dichloroethene 4.70 toluene 4.45 tion time and has a greater response than that of a corresponding reference
trans-1,2-dichloroethene 4.70 m-xylene 6.51 material, then Procedure B is performed for verification of the analyte. In the
1,4-dioxane 1.90 o-xylene 0.98
ethylbenzene 1.84 p-xylene 1.52 second supplement of USP 30/NF 25, an exemption is made for 1,1,1-
methanol 15.00 trichloroethane, where a response greater than 150 times the peak response
In dimethyl sulfoxide, 1mL/ampul denotes an amount above the percent daily exposure limit. Figures 4 through 6
cat. # 36271 (ea.) illustrate the analysis of Class 1, Class 2 Mixture A, and Class 2 Mixture B resid-
ual solvent mixes by Procedure A. The resolution between acetonitrile and
Residual Solvents Class 2 - Mix B (8 components) dichloromethane was easily achieved using an Rtx®-1301 column.
chloroform 60µg/mL nitromethane 50
1,2-dimethoxyethane 100 pyridine 200
n-hexane (C6) 290 tetralin 100 Figure 4 USP residual solvent Class 1 standard solution on an Rtx®-1301
2-hexanone 50 trichloroethene 80 column (G43).
In dimethyl sulfoxide, 1mL/ampul
S/N
cat. # 36280 (ea.)
1. 1,1-dichloroethene >3 SYSTEM SUITABILITY
Quantity discounts not available. 2. 1,1,1-trichloroethane >5
3. carbon tetrachloride >3 CRITERIA MET
4. benzene >3
5. 1,2-dichloroethane >3
Residual Solvents Class 2 - Mix C (8 components)
2-ethoxyethanol 800µg/mL 2-methoxyethanol (methyl
ethylene glycol 3,100 Cellosolve®) 250
formamide 1,100 N-methylpyrrolidone 2,650
N,N-dimethylacetamide 5,450 sulfolane 800
N,N-dimethylformamide 4,400
In dimethyl sulfoxide, 1mL/ampul
GC_PH00909
cat. # 36273 (ea.)

All USP singles available!

Visit us online at www.restek.com Column: Rtx®-1301, 30m, 0.32mm ID, 1.8µm (cat.# 16092) Headspace Conditions
Sample: USP <467> Class 1 standard solution Instrument: Tekmar HT3
(cat.# 36279) in 20mL headspace vial Transfer line temp.: 105°C
Inj.: headspace injection (split ratio 1:5), 1mm split Valve oven temp.: 105°C
liner, Siltek® deactivated (cat.# 20972-214.1) Sample temp.: 80°C
Inj. temp.: 140°C Sample equil. time: 45 min.
Carrier gas: helium, constant flow Vial pressure: 10psi
Flow rate: 2.16mL/min., 35.3cm/sec. Pressurize time: 0.5 min.
Oven temp.: 40°C for 20 min. to 240°C @ Loop fill pressure: 5psi
10°C/min. (hold for 20 min.) Loop fill time: 2.00 min.
Det.: FID @ 240°C Inject time: 1.00 min.

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Figure 5 USP residual solvent Class 2 Mixture A standard solution on an Rtx®-1301 column (G43).

1. methanol 9. 1,4-dioxane
SYSTEM SUITABILITY CRITERIA MET 2. acetonitrile (resolution=1.35) 10. toluene
3. dichloromethane 11. chlorobenzene
4. trans-1,2-dichloroethene 12. ethyl benzene
5. cis-1,2-dichloroethene 13. m-xylene/p-xylene
6. tetrahydrofuran 14. o-xylene
7. cyclohexane
8. methylcyclohexane
2. acetonitrile (resolution = 1.35)
3. dichloromethane
Column: Rtx®-1301, 30m, 0.32mm ID, 1.8µm (cat.# 16092)
Sample: USP <467> Class 2 Mixture B standard solution
(cat.# 36280) in 20mL headspace vial
Inj.: headspace injection (split ratio 1:5), 1mm split
liner Siltek® deactivated (cat.# 20972-214.1)
Inj. temp.: 140°C
Carrier gas: helium, constant flow
9. 1,4-dioxane
Flow rate: 2.16mL/min., 35.3cm/sec.
Oven temp.: 40°C for 20 min. to 240°C @
10°C/min. (hold for 20 min.)
Det.: FID @ 240°C
Headspace Conditions
Instrument: Tekmar HT3
Transfer line temp.: 105°C
Valve oven temp.: 105°C
Sample temp.: 80°C
Sample equil. time: 45 min.
Vial pressure: 10psi
Pressurize time: 0.5 min.
Loop fill pressure: 5psi
Loop fill time: 2.00 min.
Inject time: 1.00 min.

GC_PH00910

Figure 6 USP residual solvent Class 2 Mixture B standard solution on an Rtx®-1301 column (G43).

1. hexane
2. nitromethane
3. chloroform
4. 1,2-dimethoxyethane
5. trichloroethylene
6. pyridine
7. 2-hexanone
8. tetralin

Column: Rtx®-1301, 30m, 0.32mm ID, 1.8µm (cat.# 16092)

Sample: USP <467> Class 2 Mixture B standard solution
(cat.# 36280) in 20mL headspace vial
Inj.: headspace injection (split ratio 1:5), 1mm split
liner Siltek® deactivated (cat.# 20972-214.1)
Inj. temp.: 140°C
Carrier gas: helium, constant flow
Flow rate: 2.16mL/min., 35.3cm/sec.
Oven temp.: 40°C for 20 min. to 240°C @
10°C/min. (hold for 20 min.)
Det.: FID @ 240°C
Headspace Conditions
Instrument: Tekmar HT3
Transfer line temp.: 105°C
Valve oven temp.: 105°C
Sample temp.: 80°C
Sample equil. time: 45 min.
Vial pressure: 10psi
Pressurize time: 0.5 min.
Loop fill pressure: 5psi
Loop fill time: 2.00 min.
Inject time: 1.00 min.

GC_PH00911

•5• www.restek.com
Achieving USP<467> Compliance (continued from page 5)
Procedure B - Confirmation
Once a residual solvent is identified and found to be above the percent daily
Capillary Column—Procedure A exposure limit, Procedure B is performed to confirm analyte identity. A G16
capillary column is used here as a confirmation column, because it yields an
Rtx®-1301 (G43) Columns (fused silica) alternate selectivity compared to a G43 column. The same standard and system
(Crossbond® 6% cyanopropylphenyl/94% dimethyl polysiloxane)
suitability preparations are used in Procedures A and B. The system suitability
ID df (µm) temp. limits length cat. #
0.32mm 1.80 -20 to 240°C 30-Meter 16092
requirements differ here in that the Class 1 standard solution must have a ben-
0.53mm 3.00 -20 to 240°C 30-Meter 16085 zene response greater than 5 and the resolution of acetonitrile and cis-
dichloroethene must not be less than 1 in the Class 2 Mixture A solution, a
change from the original version. If the analyte identified in Procedure A again
Capillary Column—Procedure B
Stabilwax® Columns (fused silica)
matches the retention time and exceeds the peak response of the reference mate-
rials (with the same exception to 1,1,1-trichloroethane), the analyst must quan-
(Crossbond® Carbowax® polyethylene glycol)
tify the analyte using Procedure C. Figures 7 through 9 illustrate the analysis of
ID df (µm) temp. limits length cat. #
Class 1, Class 2 Mixture A, and Class 2 Mixture B residual solvent mixes on a
Stabilwax® column. Again, the system suitability requirements were easily met.
0.32mm 0.25 40 to 250°C 30-Meter 10624
0.53mm 0.25 40 to 250°C 30-Meter 10625 Procedure C – Quantification
Once a residual solvent has been identified and verified, Procedure C is used to
quantify the analyte by analyzing the sample against compound-specific refer-
ence materials. Individual standards are prepared by diluting the analyte in solu-
tion to a concentration of 1/20 of the concentration limit given under concen-
tration limit Table 1 or 2 of the method. Following the procedure and instru-
Custom standards ment conditions in either Procedure A or B (whichever provides the most defin-
Visit us online at www.restek.com itive results), a quantifiable result is produced. For water-insoluble articles, the
same procedure is followed, except dimethylformamide or dimethylsulfoxide is
used as the diluent.

Figure 7 USP residual solvent Class 1 standard solution on a Stabilwax®

column (G16).

SYSTEM SUITABILITY CRITERIA MET

S/N
1. 1,1-dichloroethene >5
2. 1,1,1-trichloroethane >5
3. carbon tetrachloride >5
4. benzene >5
5. 1,2-dichloroethane >5

Interested in dual
column analysis?
Review our technical poster on
dual column analysis of residual
solvents.

GC_PH00951

Column: Stabilwax®, 30m, 0.32mm ID, 0.25µm Headspace Conditions

(cat.# 10624) Instrument: Overbrook Scientific
Sample: USP Stock Mixture USP<467> Residual HT200H
Solvents Class 1 Mix (cat.# 36279) in Syringe temp.: 100°C
20mL headspace vial (cat.# 24685), Sample temp.: 80°C
water diluent Sample equil. time.: 45 min.
Inj.: headspace injection (split ratio 1:5), Injection vol.: 1.0mL
2mm splitless liner IP deactivated Injection speed: setting 8
(cat.# 20712) Injection dwell: 5 sec.
Inj. temp.: 140°C
Carrier gas: helium, constant flow
Flow rate: 2.15mL/min., 35.2cm/sec.
Oven temp.: 50°C for 20 min. to 165°C @ 6°C/min.
(hold for 20 min.)
Det.: FID @ 250°C

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Figure 8 USP residual solvent Class 2 Mixture A standard solution on a Stabilwax® column (G16).

SYSTEM SUITABILITY CRITERIA MET— 1. cyclohexane

RESOLUTION BETWEEN PEAKS 7 & 8 > 1.0 2. methylcyclohexane
3. trans-1,2-dichloroethene
4. tetrahydrofuran
5. methanol
6. dichloromethane
7. cis-1,2-dichloroethene
8. acetonitrile
9. toluene
10. 1,4-dioxane
11. ethyl benzene
12. p-xylene
13. m-xylene
14. o-xylene
15. chlorobenzene

Column: Stabilwax®, 30m, 0.32mm ID, 0.25µm

(cat.# 10624)
Sample: USP Stock Standard Residual Solvents
Class 2 Mix A (cat.# 36271) in 20mL headspace
vial (cat.# 24685), water diluent
Inj.: headspace injection (split ratio 1:5), 2mm
splitless liner IP deactivated (cat.# 20712)
Inj. temp.: 140°C
Carrier gas: helium, constant flow
Flow rate: 2.15mL/min., 35.2cm/sec.
Oven temp.: 50°C for 20 min. to 165°C @ 6°C/min.
(hold for 20 min.)
Det.: FID @ 250°C

Headspace Conditions
Instrument: Overbrook Scientific HT200H
Syringe temp.: 100°C
Sample temp.: 80°C
GC_PH00952 Sample equil. time.: 45 min.
Injection vol.: 1.0mL
Injection speed: setting 8
Injection dwell: 5 sec.

Figure 9 USP residual solvent Class 2 Mixture B standard solution on a Stabilwax® column (G16).

1. hexane
2. 1,2-dimethoxyethane
3. trichloroethylene
4. chloroform
5. 2-hexanone
6. nitromethane
7. pyridine
8. tetralin

Column: Stabilwax®, 30m, 0.32mm ID, 0.25µm

(cat.# 10624)
Sample: USP Stock Standard Residual Solvents
Class 2 Mix B (cat.# 36272) in 20mL headspace
vial (cat.# 24685), water diluent
Inj.: headspace injection (split ratio 1:5), 2mm
splitless liner IP deactivated (cat.# 20712)
Inj. temp.: 140°C
Carrier gas: helium, constant flow
Flow rate: 2.15mL/min., 35.2cm/sec.
Oven temp.: 50°C for 20 min. to 165°C @ 6°C/min.
(hold for 20 min.)
Det.: FID @ 250°C

Headspace Conditions
Instrument: Overbrook Scientific HT200H
Syringe temp.: 100°C
Sample temp.: 80°C
Sample equil. time.: 45 min.
Injection vol.: 1.0mL
Injection speed: setting 8
Injection dwell: 5 sec.

GC_PH00953

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 Optimize Your Testing Procedure
Tools, Tips, & Techniques for Improving Method Performance
Implementing the revised method for USP<467> can be difficult if the instru-
Use Smaller Bore Liners for ment is not optimized correctly. Key issues to address when setting up headspace
Better Efficiency GC systems include minimizing system dead volume, maintaining inert sample
flow paths, and achieving efficient sample transfer. While the second supple-
1mm Split Liners for Agilent GCs ment contains a change that allows for modifications to the split ratio, column
and liner choices are critical to analytical success.
ID* x OD & Length qty. cat.#
1mm Split** Use Smaller Bore Liners for Better Resolution
1.0mm x 6.3mm x 78.5mm ea. 20972 The function of an injection port in headspace analysis is very different than in
1.0mm x 6.3mm x 78.5mm 5-pk. 20973
direct liquid injection. In direct injection, the sample is vaporized in the injec-
tion port and larger volume liners (e.g., 4mm) are typically used since the liner
2mm Splitless Liners for Agilent GCs must be able to accommodate the solvent expansion volume. In contrast, in
headspace analysis, the sample is vaporized inside the headspace vial and the
ID* x OD & Length qty. cat.# resulting gas sample is simply transferred into the injection port via a transfer
2mm Splitless line or syringe injection. Since solvent vaporization does not occur in the liner,
2.0mm x 6.5mm x 78.5mm ea. 20712 a large volume liner is not needed and, in fact, the use of one can cause delete-
2.0mm x 6.5mm x 78.5mm 5-pk. 20713
2.0mm x 6.5mm x 78.5mm 25-pk. 20714
rious effects such as band broadening and decreased peak efficiency. For head-
space applications, a smaller bore liner, preferably 1mm, is recommended. The
smaller liner volume reduces band broadening by increasing linear velocity in
Split Liners for Varian 1075/1077 GCs the liner allowing faster sample transfer and improving resolution (Figure 10).

ID* x OD & Length qty. cat.#

Figure 10 Improve system suitability pass rates using smaller bore liners.
1mm Split
1.0mm x 6.3mm x 72mm ea. 20970 2
1.0mm x 6.3mm x 72mm 5-pk. 20971

Resolution passes if using

Split Liners for Shimadzu GCs a 1mm liner (red line), but
fails with a 4mm liner
ID* x OD & Length qty. cat.# 1. acetonitrile
(black line). 2. dichloromethane
1mm Split
1.0mm x 5.0mm x 95mm ea. 20976
1.0mm x 5.0mm x 95mm 5-pk. 20977
1.0mm x 5.0mm x 95mm 25-pk. 20978

Resolution = 1.35 for

SPME Liners for Shimadzu 17A, 2010, the 1mm liner
and 2014 GCs
ID* x OD & Length qty. cat.#
SPME Liner 1
.75mm x 5.0mm x 95mm ea. 22278 GC_PH00912
.75mm x 5.0mm x 95mm 5-pk. 22279
4.30 4.40 4.50 4.60 4.70 4.80
Time (min)

Zero Dilution Liners for PerkinElmer Auto SYS™

and Clarus GCs Speed Up Method Development Using a Retention Time Index
ICH guideline Q3C states that residual solvents need only be tested when pro-
ID* x OD & Length qty. cat.#
Zero Dilution Inner Liner
duction or purification processes are known to result in the presence of such sol-
1.0mm x 2.0mm x 73mm ea. 22990 vents. Therefore, in many cases exhaustive testing is not needed and individual
1.0mm x 2.0mm x 73mm 5-pk. 22991 validated methods for smaller, specific analyte lists are an option. To simplify
column selection and reduce method development time, Restek has created a
Zero Dilution Outer Liner
retention time index for ICH Class 1, 2, and 3 residual solvents on various phas-
2.5mm x 6.2mm x 90mm ea. 22992
2.5mm x 6.2mm x 90mm 5-pk. 22993 es (Table I). To use this index, simply locate the analytes of interest on the list
and determine which phase gives the optimal amount of resolution—or differ-
*Nominal ID at syringe needle expulsion point.
**Use this liner for increased sensitivity.
ence in retention time—between your target compounds. A critical coelution is
indicated by a failure to achieve a retention time difference of greater than 1.5
minutes.

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Table I Reduce method development time—use a retention time index for column selection.
Retention time data collected using the following conditions:
G16 Stabilwax®: 30m, 0.25mm ID, 0.5µm df, Phase ratio: 125, Oven program: 40ºC, hold 1 min., to 190ºC @ 4ºC/min., hold 15 min., Carrier flow: 1.2mL/min., Dead time: 1.38 min. @ 45ºC
G16 Rtx®-WAX: 30m, 0.25mm ID, 0.5µm df, Phase ratio: 125, Oven program: 40ºC, hold 1 min., to 190ºC @ 4ºC/min., hold 15 min., Carrier flow: 1.2mL/min., Dead time: 1.40 min. @ 45ºC
G43 Rtx®-1301: 30m, 0.25mm ID, 1.0µm df, Phase ratio: 63, Oven program: 40ºC, hold 1 min., to 190ºC @ 4ºC/min., hold 15 min., Carrier flow: 1.2mL/min., Dead time: 1.40 min. @ 45ºC
G27 Rxi®-5ms: 30m, 0.25mm ID, 1.0µm df, Phase ratio: 63, Oven program: 40ºC, hold 1 min., to 190ºC @ 4ºC/min., hold 15 min., Carrier flow: 1.1mL/min., Dead time: 1.49 min. @ 45ºC
G1 Rtx®-1: 60m, 0.53mm ID, 3.00µm df, Phase ratio: 43, Oven program: 30ºC, hold 4 min., to 220ºC @ 4ºC/min., Carrier flow: 6.3mL/min., Dead time: 2.54 min. @ 35ºC
Rtx®-200: 60m, 0.53mm ID, 3.00µm df, Phase ratio: 43, Oven program: 30ºC, hold 4 min., to 220ºC @ 4ºC/min., Carrier flow: 7.8mL/min., Dead time: 2.22 min. @ 35ºC
G16 G16 G43 G27 G1 NA
Carrier gas: helium ICH Stabilwax® Rtx®-WAX Rtx®-1301 Rxi®-5ms Rtx®-1 Rtx®-200
Compound Class Retention Time Retention Time Retention Time Retention Time Retention Time Retention Time
1,1,1-trichloroethane 1 3.96 3.49 5.43 5.40 10.82 8.35
1,1,2-trichloroethene 2 15.72 14.28 10.99 9.77 16.75 14.94
1,1-dichloroethene 1 2.23 2.04 2.79 4.41 5.73 4.16
1,2-dichloroethane 1 8.80 7.68 6.15 5.46 10.38 9.74
cis-1,2-dichloroethene 2 6.50 5.65 4.79 2.88 8.71 7.11
trans-1,2-dichloroethene 2 3.63 3.20 3.55 3.54 7.17 5.16
1,2-dimethoxyethane 2 4.80 4.18 6.03 5.54 10.98 10.63
1,4-dioxane 2 8.55 7.49 7.86 7.26 13.54 14.34
1-butanol 3 11.13 10.08 7.18 5.76 11.49 10.13
1-pentanol 3 14.95 13.75 11.19 9.44 16.99 14.95
1-propanol 3 7.69 6.80 4.20 3.37 6.81 6.13
2-butanol 3 7.25 6.44 5.08 4.16 8.51 7.69
2-ethoxyethanol 2 13.99 12.70 8.69 7.36 13.91 13.99
2-methoxyethanol 2 12.42 11.11 6.02 5.14 9.83 10.74
2-methyl-1-propanol 3 9.32 8.40 6.00 4.79 * *
2-propanol 3 4.81 4.25 3.00 2.55 4.91 4.69
3-methyl-1-butanol 3 13.42 12.25 9.86 8.26 15.28 13.55
acetic acid 3 22.47 20.34 6.52 4.61 8.84 8.96
acetone 3 3.02 2.64 2.89 2.50 4.64 7.68
acetonitrile 2 6.91 5.83 3.28 2.47 4.32 8.89
anisole 3 18.65 17.09 17.12 16.28 25.00 22.84
benzene 1 5.23 4.54 5.98 3.83 11.63 9.17
butyl acetate 3 8.86 7.88 12.12 11.38 19.43 19.63
carbon tetrachloride 1 3.96 3.49 5.61 5.90 11.89 7.42
chlorobenzene 2 13.91 12.54 13.55 13.14 21.56 18.48
chloroform 2 7.31 6.41 5.23 4.64 9.18 6.66
cumene 3 12.36 11.17 16.66 16.69 25.88 20.90
cyclohexane 2 2.16 2.01 5.37 5.89 * *
dichloromethane 2 5.01 4.33 3.31 3.06 5.87 4.88
dimethylsulfoxide 3 26.47 24.43 16.62 13.01 18.81 30.95
ethanol 3 4.98 4.37 2.52 2.19 4.03 3.80
ethyl acetate 3 4.08 3.56 4.87 4.44 9.04 10.35
ethyl benzene 2 10.72 9.58 13.86 13.81 22.54 18.18
ethyl ether 3 1.72 1.63 2.58 2.67 5.34 3.87
ethyl formate 3 3.16 2.78 3.00 2.78 5.46 6.48
ethylene glycol 2 28.06 26.23 10.77 6.63 12.59 13.86
formamide 2 32.99 30.93 11.85 7.30 12.72 19.93
formic acid 3 24.64 22.09 5.19 2.60 5.59 5.06
heptane 3 1.98 1.86 6.34 6.98 14.18 7.84
hexane 2 1.65 1.58 3.77 4.11 9.06 4.86
isobutyl acetate 3 6.99 6.18 10.39 9.69 17.35 18.02
isopropyl acetate 3 4.26 3.74 6.19 5.71 11.47 12.38
methanol 2 4.23 3.64 1.96 1.80 3.14 2.93
methyl acetate 3 3.19 2.80 3.17 2.93 5.80 7.10
methylbutyl ketone 2 9.10 8.05 11.81 10.50 17.94 20.81
methylcyclohexane 2 2.50 2.30 7.31 7.95 15.49 9.21
methylethyl ketone 3 4.33 3.76 4.90 4.09 7.99 11.55
methylisobutyl ketone 3 6.84 5.97 9.64 8.49 15.35 18.41
m-xylene 2 11.21 10.04 15.46 14.17 23.01 18.78
N,N-dimethylacetamide 2 20.75 19.01 12.95 13.96 21.42 30.00
N,N-dimethylformamide 2 18.04 16.26 13.09 10.23 16.52 26.19
nitromethane 2 11.82 10.31 4.84 3.53 6.30 12.01
N-methylpyrrolidone 2 29.84 27.86 25.09 21.85 29.99 38.08
o-xylene 2 12.79 11.51 15.46 15.26 24.23 20.33
pentane 3 1.49 1.45 2.39 2.62 5.36 3.29
propyl acetate 3 5.98 5.29 8.03 7.44 * *
p-xylene 2 10.98 9.82 14.29 15.27 22.99 18.69
pyridine 2 12.64 11.24 9.60 8.57 15.40 16.45
sulfolane 2 47.62 43.31 34.02 28.90 36.76 48.67
tert-butylmethyl ether 3 1.94 1.82 3.50 3.59 7.52 5.73
tetrahydrofuran 3 3.63 3.19 5.12 4.90 9.81 9.48
tetralin 2 25.12 23.48 27.49 27.44 37.27 31.72
toluene 2 7.86 6.91 9.80 9.66 17.36 14.00
1,1-diethoxypropane — 5.42 4.84 11.39 11.38 19.82 15.08
2,2-dimethoxypropane — 3.11 2.79 5.48 5.55 11.37 8.67
2-chloropropane — 1.96 1.82 2.67 2.66 5.20 4.61
2-methylpentane — 1.58 1.52 3.22 3.56 7.72 4.32
acetaldehyde — 2.05 1.85 1.86 1.84 3.14 3.90
chloroethane — 1.83 1.71 2.14 2.10 3.97 3.55
chloromethane — 1.63 1.55 1.70 1.70 3.01 2.73
ethylene oxide — 2.05 1.86 1.89 2.02 3.59 3.92
formaldehyde — 2.25 1.57 1.68 1.58 2.66 2.59
isoamyl acetate — 10.51 9.43 14.84 14.18 22.80 22.62
isooctane — 1.85 1.75 5.84 6.59 13.66 8.07
isopropyl ether — 1.86 1.76 4.03 4.23 9.03 5.83
methyl cyclopentane — 1.91 1.79 4.50 4.93 10.41 5.81
methyl isopropyl ketone — 4.93 4.29 6.58 5.69 11.04 14.47
methylal — 2.26 2.06 2.84 2.82 5.65 5.09
trichloroethene — 6.50 5.70 7.07 7.05 13.58 9.75
water — 8.24 7.18 1.74 1.68 2.75 2.57
* Not determined

•9• www.restek.com
 Restek Offers An Extensive Selection of Capillary Columns
For Successful Method Development & Validation
G43 G27
Rtx®-624 Columns (fused silica) Rxi®-5ms Columns (fused silica)
®
(Crossbond 6% cyanopropylphenyl/94% dimethyl polysiloxane) ®
(Crossbond 5% diphenyl/95% dimethyl polysiloxane)

ID df (µm) temp. limits 30-Meter 60-Meter ID df (µm) temp. limits 30-Meter 60-Meter
0.25mm 1.40 -20 to 240°C 10968 10969 0.25mm 0.50 -60 to 330/350°C 13438 13441
0.32mm 1.80 -20 to 240°C 10970 10972 1.00 -60 to 330/350°C 13453 13456
0.53mm 3.00 -20 to 240°C 10971 10973 0.32mm 0.50 -60 to 330/350°C 13439 13442
ID df (µm) temp. limits 20-Meter 40-Meter 1.00 -60 to 330/350°C 13454 13457
free literature 0.18mm 1.00 -20 to 240°C 40924 40925 0.53mm 1.00 -60 to 330/350°C 13455
1.50 -60 to 330/350°C 13470
ID df (µm) temp. limits 20-Meter
0.18mm 0.18 -60 to 330/350°C 13402

Rtx®-1301 Columns (fused silica) G43 0.30 -60 to 330/350°C 13409

0.36 -60 to 330/350°C 13411
(Crossbond® 6% cyanopropylphenyl/94% dimethyl polysiloxane)
ID df (µm) temp. limits* 30-Meter 60-Meter
0.25mm 0.50 -20 to 270°C 16038 16041
G1
1.00 -20 to 260°C 16053 16056 Rtx®-1 Columns (fused silica)
1.40 -20 to 240°C 16016 (Crossbond® 100% dimethyl polysiloxane)
0.32mm 0.50 -20 to 270°C 16039 16042
ID df (µm) temp. limits 30-Meter 60-Meter
1.00 -20 to 260°C 16054 16057
0.25mm 0.50 -60 to 330/350°C 10138 10141
1.50 -20 to 250°C 16069 16072
1.00 -60 to 320/340°C 10153 10156
Genuine Restek 1.80 -20 to 240°C 16092 16093
0.32mm 1.00 -60 to 320/340°C 10154 10157
Replacement Parts 0.53mm 0.50 -20 to 270°C 16040 16043
1.50 -60 to 310/330°C 10169 10172
1.00 -20 to 260°C 16055 16058
Use our handy new Genuine 3.00 -60 to 280/300°C 10184 10187
1.50 -20 to 250°C 16070 16073
Restek Replacement Parts 4.00 -60 to 280/300°C 10198
3.00 -20 to 240°C 16085 16088
(GRRP) mini-catalogs to help 5.00 -60 to 260/280°C 10178 10180
you select the supplies and 0.53mm 1.50 -60 to 310/330°C 10170 10173
replacement parts you need 3.00 -60 to 270/290°C 10185 10188
for your specific GC. We now 5.00 -60 to 270/290°C 10179 10183
have customized GRRP mini- G16 7.00 -60 to 240/260°C 10192 10193
Stabilwax® Columns (fused silica) ID df (µm) temp. limits 20-Meter 40-Meter
catalogs for each major (Crossbond® Carbowax® polyethylene glycol)
instrument manufacturer to 0.18mm 0.20 -60 to 330/350°C 40102 40103
simplify your product search. ID df (µm) temp. limits 30-Meter 60-Meter 0.40 -60 to 320/340°C 40111 40112
Download these and other 0.25mm 0.25 40 to 250°C 10623 10626
pieces from our website at 0.50 40 to 250°C 10638 10641
www.restek.com/grrp. 0.32mm 0.25 40 to 250°C 10624 10627
0.50 40 to 250°C 10639 10642 Rtx®-200 Columns (fused silica)
For Agilent GCs 1.00 40 to 240/250°C 10654 10657 (Crossbond® trifluoropropylmethyl polysiloxane)
(lit. cat.# 59627F) 0.53mm 1.00 40 to 240/250°C 10655 10658 ID df (µm) temp. limits* 30-Meter 60-Meter
1.50 40 to 230/240°C 10669 10672 0.25mm 0.50 -20 to 310/330°C 15038 15041
For Agilent 5890 GCs
2.00 40 to 220/230°C 10670 1.00 -20 to 290/310°C 15053 15056
(lit. cat.# 580216)
0.32mm 1.00 -20 to 290/310°C 15054 15057
For PerkinElmer GCs 1.50 -20 to 280/300°C 15069 15072
(lit. cat.# 580038)
also available 0.53mm 1.00
1.50
-20 to 290/310°C
-20 to 280/300°C
15055
15070
15058
15073
For Shimadzu GCs Custom Column Lengths: 3.00 -20 to 260/280°C 15085 15088
(lit. cat.# 580037) If you do not see the column dimension you need, call our ID df (µm) temp. limits 20-Meter 40-Meter
customer service team, and we will make the column for you. 0.18mm 0.20 -20 to 310/330°C 45002 45003
For Thermo Scientific GCs
0.40 -20 to 310/330°C 45011 45012
(lit. cat.# 580039)

For Varian GCs *Maximum temperatures listed are for 15- and 30-meter lengths. Longer lengths may have a slightly reduced maximum temperature.
(lit. cat.# 59224A)

www.restek.com • 10 •
 Simplify Lab Work with Innovative Accessories
Dual Vespel® Ring Inlet Seals for Agilent GCs
• Vespel® ring embedded in bottom surface eliminates need for washer.
• Vespel® ring embedded in top surface reduces operator variability by requiring minimal torque to seal.
• Prevents oxygen from permeating into the carrier gas, increasing column lifetime.
Washerless, leak-tight seals for Agilent GCs
0.8mm ID Dual Vespel Ring Inlet Seal 2-pk. /price 10-pk. /price
Gold-Plated 21240 21241
Siltek Treated 21242 21243
Stainless Steel 21238 21239 Patented.
1.2mm ID Dual Vespel Ring Inlet Seal 2-pk./price 10-pk./price
Gold-Plated 21246 21247
Siltek Treated 21248 21249
Stainless Steel 21244 21245

Dual Vespel® Ring Cross-Disk Inlet Seals for Agilent GCs

• Ideal for high-flow split applications.
• Washerless, leak-tight seals.
0.8mm ID Dual Vespel Ring Cross-Disk Inlet Seal 2-pk./price 10-pk. /price
Gold-Plated 22083 22084
Siltek Treated 22085 22086
Stainless Steel 22087 22088

Injection Port Weldments for Agilent GCs

Easily attach your autosampler with pre-installed low dead volume fittings. A

For Agilent GCs with Tekmar Transfer Lines

Description qty. cat.#
A) Weldment for Agilent 6890 GCs ea. 22664
Weldment for Agilent 6890 GCs with optional canister filter ea. 22668
Weldment for Agilent 5890 GCs ea. 22666
For Agilent GCs with OI Purge and Trap Systems
Description qty. cat.#
B) Weldment for Agilent 6890 GCs ea. 22665
Weldment for Agilent 6890 GCs with optional canister filter ea. 22669
Weldment for Agilent 5890 GCs ea. 22667
B

FID Replacement Jets

Standard Version High-Performance Version
• Engineered with a fluted tip to guide the • Similar to the standard version, but Siltek® treated.
capillary column into the jet. • Extremely inert, for use with active compounds.
• Threads specially coated for easy installation
and removal.
• Special processing ensures the highest degree
of cleanliness.
Capillary Adaptable FID Replacement Jet for Agilent 5890/6890/6850 GCs
Similar to
0.011-Inch ID Tip Agilent part # qty. cat.# qty. cat.#
Standard, 0.011-Inch ID Tip 19244-80560 ea. 20670 3-pk. 20671
High-Performance Siltek Treated, 0.011-Inch ID Tip 19244-80560 ea. 20672 3-pk. 20673
did you know?
Capillary Dedicated FID Replacement Jet for Agilent 6890/6850/7890 GCs
Restek carries a full line of
Similar to
FID replacement jets. Visit
0.011-Inch ID Tip Agilent part # qty. cat.# qty. cat.#
www.restek.com for a
Standard, 0.011-Inch ID Tip G1531-80560 ea. 21621 3-pk. 21682
complete selection.
High-Performance Siltek Treated, 0.011-Inch ID Tip G1531-80560 ea. 21620 3-pk. 21683

• 11 • www.restek.com
 Direct Replacement FID Collector Assembly Kit for Agilent 6890/6850/7890 GCs
• Constructed of high-quality stainless steel.
A • Meets or exceeds manufacturer’s performance.
Description Similar to Agilent part # qty. cat.#
4 A) FID Collector Assembly Kit (includes insulator) G1531-60690 kit 21699
3
FID Collector Assembly Kit w/Siltek Ignitor Castle — kit 21132

Replacement FID Parts for Agilent 6890/6850/7890 GCs

• Meets or exceeds manufacturer’s performance.
2 Description Similar to Agilent part # qty. cat.#
1) FID Collector (includes insulators) G1531-20690 G1531-20700 ea. 21139
1 2) FID Collector Nut and Washer 19231-20940 5181-3311 set 21136
3) FID Ignitor* 19231-60680 ea. 21001
4) FID Ignitor Castle 19231-20910 ea. 21137
Siltek FID Ignitor Castle — ea. 21135
*Also fits OI Analytical 4410 detector (similar to OI part # 191833).

The New Restek Electronic Leak Detector!

We are pleased to introduce the new, enhanced Restek Electronic Leak Detector. With our new unit
you’ll receive the great performance that you’ve come to trust from our current Leak Detector; but
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• Rugged side grips for added durability.
tech tip • Handy probe storage for cleanliness.
Avoid using liquid leak • Longer battery lifetime.
detectors on a capillary • Automatic shut-off capabilities.
system! Liquids can be drawn • A convenient carrying and storage case.
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plugs included).

Backed by a 1 year warranty, the new Restek Leak Detector will

again set an industry standard for performance and affordability
Restek Trademarks: in a hand-held Leak Detector.
Crossbond, Rtx, Rxi, Siltek,
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Restek logo. We will have units available for delivery in July 2008. Don’t miss
this opportunity to reserve your new Leak Detector. Call Restek
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Technology Corp.), Freon, Description qty cat.#
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Order your unit today! 1-800-356-1688, ext. 3

Restek Corporation Presorted Standard

110 Benner Circle US Postage
Bellefonte, PA 16823-8812 PAID
Restek

Lit. Cat.# PHFL1018

© 2008 Restek Corporation.
Restek Environmental Products
Innovative Solutions, Comprehensive Support

Chromatography Products
www.restek.com
 Volatiles
Volatile organic compounds (VOCs) are usually analyzed using a purge and trap system connected to a GC. The column used
must have a selective stationary phase to resolve the volatile pollutants, have a sufficient film thickness to retain and resolve the low
boiling volatile compounds (i.e., dichlorodifluoromethane), and must be thermally stable to elute the high boiling volatiles com-
pounds (i.e., hexachlorobutadiene & naphthalene).
The first fused silica columns used for analyzing volatiles were based on diphenyl/dimethyl polysiloxane stationary phases.
However, resolution of gases has always been problematic with these phases. Restek designed the Rtx®-VMS column specifically to
optimize separation of volatiles in the most commonly used EPA volatiles methods. A faster oven ramp rate is possible because
these compounds elute farther apart on the Rtx®-VMS phase, eliminating partial coelutions that interfere with quantification.
Using the EPA suggested surrogates (i.e., chlorobenzene-d5) analysis time can be less than 10 minutes with a narrow bore column,
allowing you to connect two purge and trap units to one GC/MS instrument – significantly increasing sample throughput.

Figure 1 Excellent resolution of bromomethane and chloroethane, as well as challenging isomer pairs like
2-/4-chlorotoluene on the Rtx®-VMS column.
1. dichlorodifluoromethane 24. bromochloromethane 47. n-propyl acetate 70. o-xylene 84. 1,2,4-trimethylbenzene
2. chloromethane 25. chloroform 48. 2-chloroethanol (2500ppb) 71. stryrene 85. sec-butylbenzene
3. vinyl chloride 26. ethyl acetate 49. cis-1,3-dichloropropene 72. bromoform 86. p-isopropyltoluene
4. bromomethane 27. carbon tetrachloride 50. toluene-d8 (SMC) 73. isopropylbenzene 87. 1,3-dichlorobenzene
5. chloroethane 28. methyl acrylate 51. toluene 74. 4-bromo-1-fluorobenzene (SMC) 88. 1,4-dichlorobenzene-d4 (IS)
6. trichlorofluoromethane 29. propargyl alcohol (500ppb) 52. pyridine (250ppb) 75. bromobenzene 89. 1,4-dichlorobenzene
7. ethanol (2500ppb) 30. dibromofluoromethane (SMC) 53. tetrachloroethene 76. n-propylbenzene 90. n-butylbenzene
8. 1,1-dichloroethene 31. tetrahydrofuran 54. 4-methyl-2-pentanone 77. 1,1,2,2-tetrachloroethane 91. 1,2-dichlorobenzene
9. carbon disulfide (40ppb) 32. 1,1,1-trichloroethane 55. trans-1,3-dichloropropene 78. 2-chlorotoluene 92. 1,2-dibromo-3-chloropropane
10. allyl chloride 33. 2-butanone 56. 1,1,2-trichloroethane 79. 1,3,5-trimethylbenzene 93. nitrobenzene (250ppb)
11. methylene chloride 34. 1,1-dichloropropene 57. ethyl methacrylate 80. 1,2,3-trichloropropane 94. hexachlorobutadiene
12. acetone 35. benzene 58. dibromochloromethane 81. 4-chlorotoluene 95. 1,2,4-trichlorobenzene
13. trans-1,2-dichloroethene 36. pentafluorobenzene (IS) 59. 1,3-dichloropropane 82. tert-butylbenzene 96. naphthalene
14. methyl tert-butyl ether 37. tert-amyl-methyl ether 60. 1,2-dibromoethane 83. pentachloroethane 97. 1,2,3-trichlorobenzene
15. tert-butyl alcohol (100ppb) 38. 1,2-dichloroethane 61. n-butyl acetate
16. diisopropyl ether 39. isobutyl alcohol (500ppb) 62. 2-hexanone
79,80
17. 1,1-dichloroethane 40. isopropyl acetate 63. 2-picoline (250ppb)
18. acrylonitrile 41. trichloroethene 64. chlorobenzene-D5 (IS)
82,83 88,89 96
19. vinyl acetate 42. 1,4-difluorobenzene (SMC) 65. chlorobenzene 86 90
20. allyl alcohol (250ppb) 43. dibromomethane 66. ethylbenzene 68,69
21. ethyl-tert-buyl ether 44. 1,2-dichloropropane 67. 1,1,1,2-tetrachloroethane 85
22. cis-1,2-dichloroethene 45. bromodichloromethane 68. m-xylene
71,72 84 91 97
23. 2,2-dichloropropane 46. methyl methacrylate 69. p-xylene 76 87 95
73 81
78
restek 66,67

64,65
94

innovation! 70
75
77
• First choice for use with dual purge & traps¹
54,55
• EPA recommended surrogate used. 59
51 56 92
29-32 35 49
8 24
11 26-28 44 53
13 23 33,34 41 58 74
45 60
12 22 25 38 43 61
1 17 50
3 6 9 10 19-21 57
62,
14 36 37 40 42 46 47
2 45 16 18 63
15 48 52 93
7 39

min. 2 4 6 8 10
GC_EV00428

Column: Rtx®-VMS 20m, 0.18 mm ID, 1.00µm (cat.# 49914) Interface: 0.53mm ID Silcosteel® tubing transfer line
Conc.: 10ppb in 5mL of RO water 1:40 split at injection port. 1mm ID liner.
unless otherwise noted; ketones at 2.5X Oven temp.: 50°C (hold 4 min.) to 100°C @ 18°C/min. (hold 0 min.)
Concentrator: Tekmar LSC-3100 Purge and Trap to 230°C @ 40°C/min. (hold 3 min.)
Trap: Vocarb 3000 (type K) Carrier gas: helium @ ~1.0mL/min. constant flow
Purge: 11 min. @ 40mL/min. (ambient temperature) Adjust dichlorodifluoromethane to a retention time of 1.03
Dry purge: 1 min. @ 40mL/min. min. @ 50°C.
Desorb preheat: 245°C Detector: Agilent 5973 MSD
Desorb: 250°C for 2 min., flow 40mL/min. Scan range: 35-300amu
Bake: 260°C for 8 min.

¹A.L. Hilling and G. Smith, Environmental Testing & Analysis, 10(3), 15-19, 2001.

Rtx®-VMS Columns (fused silica)

Recommended Column (proprietary Crossbond® phase)
ID df (µm) temp. limits length cat. # price
0.18mm 1.00 -40 to 240/260°C 20-Meter 49914 $420

2
Analytical Reference Materials Reduce Dead Volume,
Contamination, & Cold Spots
8260A Internal Standard Mix
chlorobenzene-d5 fluorobenzene
1,4-dichlorobenzene-d4 The injection port can be a source for dead volume, which is especially critical when deal-
2,500µg/mL each in P&T methanol, 1mL/ampul
ing with a sample in the gas phase. The severity of the problem is a combination of the
cat. # 30241 (ea.) $25 inside diameter of the injection port liner and the total desorb flow through the port. To
reduce dead volume in the injection port, use a 1mm ID inert split liner. Always be sure to
use insulation where the transfer line attaches to the inlet line since this is a cold spot that
will condense high molecular weight analytes.
8260 Internal Standard Mix
chlorobenzene-d5 1,4-difluorobenzene Transfer lines often are the first place contamination occurs. When the response factor for
1,4-dichlorobenzene-d4 pentafluorobenzene bromoform fails the method criteria, changing the transfer line is the first step to getting
2,500µg/mL each in P&T methanol, 1mL/ampul the system working again. Replace your transfer line with our Siltek® deactivated tubing,
cat. # 30074 (ea.) $25 for optimum performance.

1mm Split Inlet Liner for Agilent GCs

8260A Surrogate Mix
ID*/OD & Length (mm) cat.#/price ea. cat.# /price 5-pk.
4-bromofluorobenzene 1,2-dichloroethane-d4
dibromofluoromethane toluene-d8 1.0 ID 6.3 OD x78.5 20972 $26 20973 $75
2,500µg/mL each in P&T methanol, 1mL/ampul *Nominal ID at syringe needle expulsion point.
cat. # 30240 (ea.) $28 Also available with Siltek® deactivation, upon request.

8260 Surrogate Mix

4-bromofluorobenzene toluene-d8
dibromofluoromethane Siltek®/Sulfinert® Treated Coiled
2,500µg/mL each in P&T methanol, 1mL/ampul 304 Grade Stainless Steel Tubing
cat. # 30073 (ea.) $28 Our most popular grade of tubing.
• chromatography applications.
• gas delivery systems.
8260B MegaMix® Calibration Mix (76 components) • lower pressures.
Please visit us online for compound list
• inert applications.
2,000µg/mL each in P&T methanol, 1mL/ampul
cat. # 30633 (ea.) $128
Price-per-foot
ID OD cat.# 5-24 ft. 25-199 ft. 200-399 ft. >4400 ft.
1
8260B MegaMix® Calibration Mix Kit 0.040" (1.02mm) /16" (1.59mm) 22505 $10.40/ft. $6.50/ft. $4.70/ft. $3.90/ft.
30633: 8260B MegaMix® *0.020" wall thickness
30265: 2-chlorethyl vinyl ether
An extra charge is applied for cutting Siltek®/Sulfinert®, Silcosteel®, or Silcosteel®-CR
Contains 1mL each of these mixtures.
tubing, calculated from the total number of pieces produced for each line item.
cat. # 30475 (kit) $137

502.2 Calibration Mix #1 (gases)

bromomethane dichlorodifluoromethane (CFC-12)
chloroethane trichlorofluoromethane (CFC-11)
chloromethane vinyl chloride free literature
200µg/mL each in P&T methanol, 1mL/ampul Optimizing the Analysis of Volatile Organic Compounds
cat. # 30439 (ea.) $26 lit. cat.# 59887A
2,000µg/mL each in P&T methanol, 1mL/ampul
cat. # 30042 (ea.) $36 Contact your Restek representative, to request your free copy!

VOA Calibration Mix #1 (ketones)

acetone 2-hexanone
2-butanone 4-methyl-2-pentanone
5,000µg/mL each in P&T methanol:water (90:10), 1mL/ampul
cat. # 30006 (ea.) $25

California Oxygenates Mix

diisopropyl ether 2,000µg/mL tert-butyl alcohol 10,000
ethyl-tert-butyl ether 2,000 methyl tert-butyl ether 2,000
tert-amyl methyl ether 2,000
In P&T methanol, 1mL/ampul
cat. # 30465 (ea.) $28

3
 Semivolatiles
Semivolatile analysis is a challenging area covering a wide range of compound classes – neutral, acidic, and basic compounds, includ-
ing anilines, phenols, PAHs, and more – that differ in both volatility and reactivity. While the chromatography is complicated by a
broad list of target analytes, many problems can be avoided by proper attention to the inlet system and an informed column choice.

Figure 1 Separate greater than 90 semivolatile compounds in less than 18 minutes, using an Rxi™-5ms column.

Excellent peak shape for

early eluting compounds
including pyridine!

Excellent resolution of benzo(b) &

benzo(k) fluoranthene!

GC_EV00823

For complete identifications, please visit www.restek.com/rxi

Column: Rxi™-5ms, 30m, 0.25mm ID, 0.25µm (cat.# 13423) Oven temp.: 50°C (hold 0.5 min.) to 265°C @ 25°C/min.,
Sample: US EPA Method 8270D mix: 8270 MegaMix™ (cat.# 31850), to 330°C @ 6°C/min. (hold 2 min.)
Benzoic Acid Standard (cat.# 31879), Benzidine Standard (cat.# 31852), Acid Surrogate Det.: Agilent 5973 GC/MS
Mix (cat.# 31025), B/N Surrogate Standard Mix (cat.# 31887), 1,4-Dioxane (cat.# 31853) Transfer line
Inj.: 1.0µL, 10ppm each analyte (10ng on column), splitless (hold 0.1 min.) temp.: 280°C
4mm Drilled Uniliner® inlet liner (hole at bottom) (cat.# 20756) Scan range: 35-550 amu
Instrument: Agilent 6890 Solvent delay: 2 min.
Inj. temp.: 250°C Tune: DFTPP
Carrier gas: helium, constant flow Ionization: EI
Flow rate: 1.2mL/min.

1. 1,4-dioxane 20. nitrobenzene-d5 40. 2-chloronaphthalene ● 60. 4-nitroanaline ● 78. 3,3’-dimethylbenzidine

2. N-nitrosodimethylamine ● 21. nitrobenzene ● 41. 2-nitroaniline ● 61. 4,6-dinitro-2-methylphenol ● 79. butyl benzyl phthalate ●
3. pyridine ● 22. isophorone ● 42. 1,4-dinitrobenzene ● 62. N-nitrosodiphenylamine 80. bis(2-ethylhexyl) adipate ●
4. 2-fluorophenol 23. 2-nitrophenol ● 43. dimethyl phthalate ● (as diphenylamine) ● 81. 3,3’-dichlorobenzidine
5. phenol-d6 24. 2,4-dimethylphenol ● 44. 1,3-dinitrobenzene ● 63. 1,2-diphenylhydrazine 82. benzo(a)anthracene ●
6. phenol ● 25. benzoic acid 45. 2,6-dinitrotoluene ● (as azobenzene) ● 83. chrysene-d12
7. aniline ● 26. bis(2-chloroethoxy)methane ● 46. acenaphthylene ● 64. 2,4,6-tribromophenol 84. chrysene ●
8. bis(2-chloroethyl) ether ● 27. 2,4-dichlorophenol ● 47. 1,2-dinitrobenzene ● 65. 4-bromophenyl phenyl ether ● 85. bis(2-ethylhexyl) phthalate ●
9. 2-chlorophenol ● 28. 1,2,4-trichlorobenzene ● 48. 3-nitroaniline ● 66. hexachlorobenzene ● 86. di-n-octyl phthalate ●
10. 1,3-dichlorobenzene ● 29. naphthalene-d8 49. acenaphthene-d10 67. pentachlorophenol ● 87. benzo(b)fluoranthene ●
11. 1,4-dichlorobenzene-d4 30. naphthalene ● 50. acenaphthene ● 68. phenanthrene-d10 88. benzo(k)fluoranthene ●
12. 1,4-dichlorobenzene ● 31. 4-chloroaniline ● 51. 2,4-dinitrophenol ● 69. phenanthrene ● 89. benzo(a)pyrene ●
13. benzyl alcohol ● 32. hexachlorobutadiene ● 52. 4-nitrophenol ● 70. anthracene ● 90. perylene-d12 ●
14. 1,2-dichlorobenzene ● 33. 4-chloro-3-methylphenol ● 53. dibenzofuran ● 71. carbazole ● 91. indeno(1,2,3-cd)pyrene ●
15. 2-methylphenol ● 34. 2-methylnaphthalene ● 54. 2,4-dinitrotoluene ● 72. di-n-butyl phthalate ● 92. dibenzo(a,h)anthracene ●
16. bis(2-chloroisopropyl) ether ● 35. 1-methylnaphthalene ● 55. 2,3,4,6-tetrachlorophenol ● 73. fluoranthene ● 93. benzo(ghi)perylene ●
17a. 4-methylphenol ● 36. hexachlorocyclopentadiene ● 56. 2,3,5,6-tetrachlorophenol ● 74. benzidine
17b. 3-methylphenol ● 37. 2,4,6-trichlorophenol ● 57. diethyl phthalate ● 75. pyrene-d10
18. N-nitroso-di-n-propylamine ● 38. 2,4,5-trichlorophenol ● 58. 4-chlorophenyl phenyl ether ● 76. pyrene ●
19. hexachloroethane ● 39. 2-fluorobiphenyl 59. fluorene ● 77. p-terphenyl-d14
●
8270 MegaMix® components

Recommended Columns
Rxi™-5ms Columns (fused silica) Rtx®-5Sil MS Columns (fused silica)
(Crossbond® 5% diphenyl / 95% dimethyl polysiloxane) (Crossbond®, selectivity similar to 5% diphenyl/95% dimethyl polysiloxane)
ID df (µm) temp. limits length cat. # price ID df (µm) temp. limits length cat. # price
0.18mm 0.18 -60 to 330/350°C 20-Meter 13402 $385 0.18mm 0.18 -60 to 330/350°C 20-Meter 42702 $380
0.18mm 0.30 -60 to 330/350°C 20-Meter 13409 $385 0.18mm 0.36 -60 to 330/350°C 20-Meter 42704 $380
0.25mm 0.25 -60 to 330/350°C 30-Meter 13423 $450 0.25mm 0.25 -60 to 330/350°C 30-Meter 12723 $470
0.25mm 0.40 -60 to 330/350°C 30-Meter 13481 $450 0.25mm 0.50 -60 to 330/350°C 30-Meter 12738 $470

4 To Order: 800-356-1688, ext. 3 www.restek.com

Analytical Reference Materials Inert Sample Path Increases Accuracy
SV Internal Standard Mix Injection port liners are designed in many configurations, four of which are commonly used
acenaphthene-d10 naphthalene-d8 for semivolatiles analysis: the single gooseneck, double gooseneck, cyclo double gooseneck,
chrysene-d12 perylene-d12 and the Drilled Uniliner®. While all four liner types are used for 8270 analysis, we recom-
1,4-dichlorobenzene-d4 phenanthrene-d10 mend the Drilled Uniliner® when using constant flow, and the cyclo double gooseneck with
2,000µg/mL each in methylene chloride, 1mL/ampul pressure pulse conditions.
cat. # 31206 (ea.) $39
4,000µg/mL each in methylene chloride, 1mL/ampul Liners shown are for Agilent instruments; liners for other instrument brands also are
cat. # 31006 (ea.) $76
available. For a complete list of liners and seals refer to our catalog or website.

Gooseneck Splitless (4mm) Cyclo Double Gooseneck (4mm)

B/N Surrogate Mix (4/89 SOW)
2-fluorobiphenyl p-terphenyl-d14
nitrobenzene-d5 4.0 ID 6.5 OD x 78.5 20799 5 pk. $85 4.0 ID 6.5 OD x 78.5 20896 5 pk. $293
1,000µg/mL each in methylene chloride, 1mL/ampul
cat. # 31024 (ea.) $27 Double Gooseneck Splitless (4mm) Drilled Uniliner (hole on bottom)
®

5,000µg/mL each in methylene chloride, 1mL/ampul

cat. # 31062 (ea.) $41 4.0 ID 6.5 OD x 78.5 20785 5 pk. $101 4.0 ID 6.3 OD x 78.5 20771 5 pk. $284
5,000µg/mL each in methylene chloride, 5mL/ampul
cat. # 31086 (ea.) $110
5,000µg/mL each in methylene chloride, 10mL/ampul
The Drilled Uniliner® is the most inert liner because the metal injection port outside the glass
cat. # 33028 (ea.) $210
liner does not contact the sample path – the sample is virtually “funneled” into the column.
Also, when using the Drilled Uniliner® inlet seals do not need to be replaced – a savings in
maintenance cost and time. The cyclo double gooseneck liner is recommended with pres-
Acid Surrogate Mix (4/89 SOW) sure pulse conditions. Its corkscrew type sample path enhances sample vaporization and
2-fluorophenol 2,4,6-tribromophenol helps prevent sample contact with metal surfaces below the liner. When using a gooseneck
phenol-d6 type liner, however, routinely replacing the inlet seal below the liner is critical. Gold plated
2,000µg/mL each in methanol, 1mL/ampul and Siltek® treated liners and seals both ensure an inert sample path, however, Siltek® treat-
cat. # 31025 (ea.) $27 ed surfaces are more resistant to abrasion during cleaning.
10,000µg/mL each in methanol, 1mL/ampul
cat. # 31063 (ea.) $41 0.8mm ID Dual Vespel® Ring Inlet Seal
10,000µg/mL each in methanol, 5mL/ampul Siltek® Treated 21242 2-pk. $58
cat. # 31087 (ea.) $110 Stainless Steel 21238 2-pk. $45
10,000µg/mL each in methylene chloride, 10mL/ampul Gold Plated 21240 2-pk. $58
cat. # 33029 (ea.) $210

GC/MS Tuning Mixture

benzidine DFTPP
4,4'-DDT pentachlorophenol restek innovation!
1,000µg/mL each in methylene chloride, 1mL/ampul
cat. # 31615 (ea.) $28 The Drilled Uniliner®
The Drilled Uniliner® provides the most inert sample pathway of all inlet liners for splitless
injection techniques. This liner connects directly to the column, eliminating contact between
the active compounds and active metal surfaces in the injector, and ensuring an inert
605 Benzidines Calibration Mix sample pathway for analyte transfer from the injection port to the column.
benzidine 3,3'-dichlorobenzidine
2,000µg/mL each in methanol, 1mL/ampul
cat. # 31030 (ea.) $28
Use hole near top configuration for
2,000µg/mL each in methylene chloride, 1mL/ampul
chlorinated pesticide analysis, when
cat. # 31834 (ea.) $28 analytes elute away from the solvent
peak, or when the sample solvent is water

8270 Matrix Spike Mix (76 components)

200µg/mL each in methanol:methylene chloride (80:20), 5mL/ampul
cat. # 31687 (ea.) $157

Use hole near bottom configuration for

8270 MegaMix® (76 components) Analytes Drilled
semivolotile analysis or when analytes
elute near the solvent peak
1,000µg/mL each in methylene chloride, 1mL/ampul, ● contact hot Uniliner® inlet
cat. # 31850 (ea.) $112 surface and liner efficiently
dead volume transfers sample
at base of onto column
●
Refer to figure for compound list splitless liner

5
 Organochlorine Pesticides and PCB
In organochlorine pesticide analysis, careful consideration of the instrument set-up and column choice can greatly improve sample
throughput – reducing costs and saving time. The most critical aspects of the inlet system are inertness and efficiency of target
analyte transfer to the analytical column. For pesticide and PCB analysis we recommend the Drilled Uniliner® for its unsurpassed
inertness (see page 5).
In the analysis shown, 20m x 0.18mm ID Rtx®-CLPesticides and Rtx®-CLPesticides2 primary and confirmation columns were
used. We connected a 5m x 0.53mm guard column to the dual analytical columns, using a SeCure™ “Y” connector kit. These
columns have been specifically designed to resolve the chlorinated pesticides when used in parallel under the same temperature
program and inlet backpressure. As shown in Figure 1, all the organochlorine pesticide compounds are baseline resolved in less
than 8 minutes.

Figure 1 Organochlorine pesticides on Rtx®-CLPesticides and Rtx®-CLPesticides2 columns.

5%Column: A: Rtx®-CLPesticides, 20m, 0.18mm ID, 0.18µm (cat.# 42102) and 1. 2,4,5,6-tetrachloro-m-xylene (surr.) 12. 4,4’ DDE
B: Rtx®-CLPesticides2, 20m, 0.18mm ID,0.14µm (cat.# 42302) with 2. α-BHC 13. dieldrin
5m x 0.53mm ID intermediate-polarity deactivated guard tubing (cat.# 10045), 3. γ-BHC 14. endrin
connected using SeCure™ “Y” Connector Kit (cat.# 20276) with 4. β-BHC 15. 4,4’ DDD
Universal “Y” Press-Tight® Connector 5. δ-BHC 16. endosulfan II
Sample: Organochlorine Pesticide Mix AB #2 (cat.# 32292), 8-80µg/mL each 6. heptachlor 17. 4,4’ DDT
component in hexane/toluene, 7. aldrin 18. endrin aldehyde
Pesticide Surrogate Mix (cat.# 32000), 200µg/mL each component in acetone 8. heptachlor epoxide 19. endosulfan sulfate
Inj.: 0.5µL splitless (hold 0.75 min.), 2mm single gooseneck inlet liner (cat.# 20796) 9. γ-chlordane 20. methoxychlor
Inj. temp.: 250°C 10. α-chlordane 21. endrin ketone
Carrier gas: helium, constant flow
Linear velocity: 20cm/sec. @ 140°C 11. endosulfan I 22. decachlorobiphenyl (surr.)
Oven temp.: 140°C (hold 1 min.) to 250°C @ 35°C/min. (hold 1 min.) to
330°C @ 35°C/min. (hold 3 min.)
Det.: ECD @ 350°C

A B

GC_EV00893 GC_EV00892

Recommended Columns
Rtx®-CLPesticides Columns (fused silica) Rtx®-CLPesticides2 Columns (fused silica)
ID df (µm) temp. limits length cat. # price ID df (µm) temp. limits length cat. # price
0.18mm 0.18 -60 to 310/330°C 20-Meter 42102 $430 0.18mm 0.14 -60 to 310/330°C 20-Meter 42302 $430
0.25mm 0.25 -60 to 320/340°C 30-Meter 11123 $480 0.25mm 0.20 -60 to 320/340°C 30-Meter 11323 $480
0.32mm 0.50 -60 to 320/340°C 30-Meter 11139 $510 0.32mm 0.50 -60 to 320/340°C 30-Meter 11325 $510
0.53mm 0.50 -60 to 300/320°C 30-Meter 11140 $565 0.53mm 0.42 -60 to 300/320°C 30-Meter 11340 $565

did you know?

We can supply all your sample extract clean-up needs.
See our catalog or website for details.

6
Analytical Reference Materials Increase Sample Throughput
Organochlorine Pesticide Mix AB #1 Using Dual Analytical Columns
(20 components)
aldrin dieldrin and a “Y” Connector Union
α-BHC endosulfan I
β-BHC endosulfan II Most laboratories need to confirm the compound identification obtained on one column
δ-BHC endosulfan sulfate
γ-BHC (lindane) endrin with a second column of different selectivity. This is best achieved by making a single
α-chlordane endrin aldehyde injection onto a guard column which is connected to two analytical columns, using a “Y”
γ-chlordane endrin ketone splitter. This allows data to be collected from both columns simultaneously, allowing sam-
4,4'-DDD heptachlor ples to be processed without waiting for the confirmation result.
4,4'-DDE heptachlor epoxide (B)
4,4'-DDT methoxychlor
200µg/mL each in hexane:toluene (1:1), 1mL/ampul Rtx®-CLPesticides Column Kits
cat. # 32291 (ea.) $46 0.25mm ID Rtx®-CLPesticides Kit cat.# 11199 (kit), $990 SAVE $89
Includes: cat.# price
30m, 0.25mm ID, 0.25µm Rtx®-CLPesticides Column 11123 $480
Organochlorine Pesticide Mix AB # 3
(20 components) 30m, 0.25mm ID, 0.20µm Rtx®-CLPesticides2 Column 11323 $480
same listing as Organochlorine Pesticide Mix AB #1, Universal Angled “Y” Press-Tight® Connector 20403 $69
shown above. 5m, 0.25mm ID Siltek® Guard Column 10026 $50
Total cost if purchased separately $1079
2,000µg/mL each in hexane:toluene (1:1), 1mL/ampul
cat. # 32415 (ea.) $71 0.32mm ID Rtx®-CLPesticides Kit cat.# 11198 (kit), $1020 SAVE $124
Includes: cat.# price
Pesticide Surrogate Mix 30m, 0.32mm ID, 0.50µm Rtx®-CLPesticides Column 11139 $510
decachlorobiphenyl 2,4,5,6-tetrachloro-m-xylene 30m, 0.32mm ID, 0.25µm Rtx®-CLPesticides2 Column 11324 $510
200µg/mL each in acetone, 1mL/ampul Universal Angled “Y” Press-Tight® Connector 20403 $69
cat. # 32000 (ea.) $25 5m, 0.32mm ID Siltek® Guard Column 10027 $55
Total cost if purchased separately $1114

Pesticide Surrogate Mix 0.53mm ID Rtx®-CLPesticides Kit cat.# 11197 (kit), $1085 SAVE $174
decachlorobiphenyl 200µg/mL Includes: cat.# price
2,4,5,6-tetrachloro-m-xylene 100 30m, 0.53mm ID, 0.50µm Rtx®-CLPesticides Column 11140 $565
In P&T methanol, 1mL/ampul 30m, 0.53mm ID, 0.42µm Rtx®-CLPesticides2 Column 11340 $565
cat. # 32453 (ea.) $25
Universal Angled “Y” Press-Tight® Connector 20403 $69
5m, 0.53mm ID IP Deactivated Guard Column 10045 $60
Organochlorine Pesticide System Evaluation Mix Total cost if purchased separately $1259
4,4'-DDT 200µg/mL endrin 100µg/mL
In MTBE, 1mL/ampul
cat. # 32417 (ea.) $25 “Y” connectors
“Y” connectors are available in both metal and glass. Glass connectors offer the best
chromatography, but are prone to leaks. To eliminate leaks we developed the SeCure™ “Y”
508.1 GC Degradation Check Mix connector, which takes advantage of our Press-Tight®
4,4'-DDT endrin connector and adds mechanical strength to hold the
100µg/mL each in ethyl acetate, 1mL/ampul columns in place. A second connector, the MXT™
cat. # 32093 (ea.) $25 “Y”-Union, is available for fused silica columns.

Technical Chlordane, Toxaphene Solutions SeCure™ “Y” - The most secure

Compound cat.# (ea.) price connector available!
1,000µg/mL in hexane, 1mL/ampul Kits include: SeCure™ “Y” connector body, 3 knurled
chlordane (technical) 32021 $23 nuts, “Y” Universal Press-Tight® union, 3 ferrules.
toxaphene 32005 $23 Ferrules Fit Column ID qty. cat.# price
2,000µg/mL in methanol, 1mL/ampul
0.25/0.28mm kit 20276 $228
chlordane (technical) 32016 $23
0.32mm kit 20277 $228
toxaphene 32015 $23
5,000µg/mL in isooctane, 1mL/ampul 0.45/0.53mm kit 20278 $228
chlordane (technical) 32072 $25
toxaphene 32071 $25
MXT™ “Y”-Union Connector Kits
for Fused Silica Columns
also available Each kit contains the MXT™ union, three 1/32-inch nuts and
three one-piece fused silica adaptors.
Aroclor® Solutions!
Description qty. cat.# price
Visit our website, see our newest catalog, or call
For 0.25mm ID Fused Silica Columns kit 21389 $129
your Restek representative for details.
For 0.32mm ID Fused Silica Columns kit 21388 $129
For 0.53mm ID Fused Silica Columns kit 21387 $129

7
 Volatile Organic Compounds in Air
One of the most widely used VOC methods for ambient air monitoring specifies sample collection with a specially prepared stain-
less steel canister, followed by GC/MS analysis. Restek can support all facets of your air monitoring program – from state-of-the-art
sampling equipment to high quality analytical reference standards.
An inert canister surface is critical to obtaining accurate sample results. Restek offers a complete line of TO-Cans™ (Summa® can-
isters) which are electropolished and extensively cleaned prior to shipping to ensure a high-quality passivated surface for improved
analyte stability. No weld marks on the spheres further reduce the occurrence of active sites. For reactive compounds, such as sul-
fur-containing components, a SilcoCan™ is your best canister choice. SilcoCan™ canisters are deactivated with Siltek® surface treat-
ment resulting in exceptional inertness and maximum sample stability, even for low level sulfur compounds.

Optional gauge
• Quickly confirm vacuum or pressure Enhanced valve and
inside canister. canister bracket
• Monitor pressure changes. Canister holder and valve
bracket protect canister,
• Fully protected by canister frame.
tube stub, and valve.
• Can be heated to 90°C during cleaning.

Siltek® tee
2-3 Port high
quality valve
Metal-to-metal seal, 2/3
turn with stainless steel
diaphragm.

We consider your TO-Cans™

and SilcoCans™ to be an
investment and offer
High-quality check-ups and reconditioning
vacuum gauge
when needed.

Serial-controlled label
For quick, sure identification.

TO-Can™ Air Monitoring Canisters

Optimized for US EPA Methods TO-14 and TO-15, and ASTM D5466
Description qty. cat.# price
6L Volume*
TO-Can™ Canister, 1/4" Valve ea. 24174 $453
TO-Can™ Canister with Gauge, 1/4" Valve ea. 24178 $610
TO-Can™ Canister with No Valve ea. 22096 $365

SilcoCan™ Air Monitoring Canisters

Ideal for low-level reactive sulfur (1-20ppb), TO-14, or TO-15 compounds
Description qty. cat.# price
6L Volume*
SilcoCan™ Canister, 1/4" Valve ea. 24182 $590
SilcoCan™ Canister, Siltek® Treated 1/4" Valve ea. 24182-650 $645
SilcoCan™ Canister with Gauge, 1/4" Valve ea. 24142 $795
SilcoCan™ Canister with Gauge, Siltek® Treated 1/4" Valve ea. 24142-650 $850
SilcoCan™ Canister with No Valve ea. 22092 $415
Replacement 1/4" Valves for Air Monitoring Canisters
1
/4" Replacement Valve (2-port) ea. 24145 $225
1
/4" Siltek® Replacement Valve (2-port) ea. 24144 $245
1
/4" Replacement Valve (3-port) ea. 24147 $235
1
/4" Siltek® Replacement Valve (3-port) ea. 24146 $260

Restek canisters are originally equipped with high-quality Parker Hannifin diaphragm valves. Each valve is helium leak-tested to 4 x
10-9cc/sec. The all-stainless steel construction eliminates contamination and withstands temperatures from -100°C to 250°C.
Compression outlet fitting, indicator plate to display open or closed position, 1/4" inlet and outlet.
*All configurations also available in 1L, 3L, and 15L volumes.

8
Recommended Columns Simplify Sampling, Increase
Rxi™-1ms Columns (fused silica) Accuracy & Efficiency
(Crossbond® 100% dimethyl polysiloxane)
ID df (µm) temp. limits length cat. # price Air Canister Heating Jacket
0.32mm 1.00 -60 to 330/350°C 60-Meter 13357 $850
Our heating jackets can help you prepare your canisters
for sampling faster and more efficiently. The jacket’s
novel design ensures complete cleaning by heating the
canister and valve together and prevents condensation,
Analytical Reference Materials ensuring more accurate results. Two temperature set-
tings, 75ºC and 150ºC. Fits all canisters up to 6L in size.
TO-15 62 Component Mix (62 components) Description qty. cat.# price
Cylinder Construction: aluminum Air Canister Heating Jacket ea. 24123 $495
Cylinder Size: 8 x 24 cm. *Not CE certified.
Volume/Pressure: 104 liters of gas @ 1800psig The ultimate in controlled heating, for reliably
Cylinder Fitting: CGA-180 outlet cleaning your air canisters!
Weight: 1.5 lbs./0.7 kg
acetone trichlorofluoromethane
benzene (Freon® 11)
benzyl chloride* dichlorodifluoromethane Passive Air Sampling Kits
bromodichloromethane (Freon® 12 )
bromoform 1,1,2-trichloro-1,2,2-trifluo Our passive sampling kits include all hardware required for field sampling (except the can-
bromomethane roethane (Freon® 113) ister) and assemble easily. Our kit was designed to reduce the number of potential leak
1,3-butadiene 1,2-dichlorotetrafluoroethane sites and is available in seven flow ranges, and in stainless steel or with Siltek® surface
2-butanone (MEK) (Freon® 114)
carbon disulfide* heptane treatment. Individual parts are also available.
carbon tetrachloride hexachloro-1,3-butadiene
chlorobenzene hexane 1. Veriflo™ SC423XL flow controller
chloroethane 2-hexanone (MBK) This flow controller is the heart of
chloroform 4-methyl-2-pentanone (MIBK) the sampling train. It is a high-quali-
chloromethane methylene chloride ty device designed to maintain a 3
cyclohexane methyl tert-butyl ether constant mass flow as the pressure
dibromochloromethane (MTBE) changes from 30" Hg to 5" Hg (we
1,2-dichlorobenzene 2-propanol recommend you stop sampling at or
1,3-dichlorobenzene propylene before 5" Hg of vacuum). All wetted
1,4-dichlorobenzene styrene
1,1-dichloroethane 1,1,2,2-tetrachloroethane parts of the flow controller can be
1,2-dichloroethane tetrachloroethene Siltek® treated.
1,1-dichloroethene tetrahydrofuran 2. Stainless steel vacuum gauge 4
cis-1,2-dichloroethene toluene Fitted to the flow controller, the
trans-1,2-dichloroethene 1,2,4-trichlorobenzene
1,2-dichloropropane 1,1,1-trichloroethane gauge monitors canister vacuum
cis-1,3-dichloropropene 1,1,2-trichloroethane change during sampling. 1 2
trans-1,3-dichloropropene trichloroethene 1
3. /4-inch Siltek sample inlet
® 5
1,4-dioxane 1,2,4-trimethylbenzene The 0.3m x 1/4-inch tubing includes a
ethanol* 1,3,5-trimethylbenzene
ethyl acetate vinyl acetate stainless steel nut on the inlet end,
ethyl benzene vinyl chloride to prevent water droplets from
ethylene dibromide m-xylene accumulating at the edge of the tub-
(1,2-dibromoethane) o-xylene ing, where they could be pulled into
4-ethyltoluene p-xylene the sampling train.
In nitrogen, 104 liters @ 1800psig 4. 2-micron frit filter and washer
1ppm cat. # 34436 (ea.) $3600 Located prior to the critical orifice to All fitting connections are 1/4"
100ppb cat. # 34437 (ea.) $3800 prevent airborne particles from tube, except where noted.
1
/4" NPT
*Stability of this compound cannot be guaranteed. clogging the critical orifice.
Replaceable. Available in stainless
steel, or Siltek® treated for optimum See our catalog for other canister
TO-14A Internal Standard/Tuning Mix inertness. volumes and sampling times.
Cylinder Construction: aluminum
5. Interchangeable critical orifice
Cylinder Size: 8 x 24 cm.
An interchangeable ruby critical orifice allows you to control the flow with very high precision.
Volume/Pressure: 104 liters of gas @ 1800psig
To select the correct critical orifice for your sample, see table below. Available in stainless steel,
Cylinder Fitting: CGA-180 outlet or Siltek® treated for optimum inertness.
Weight: 1.5 lbs./0.7 kg
Sampling Time Flow Orifice Siltek® Treated Stainless Steel
bromochloromethane chlorobenzene-d5
1-bromo-4-fluorobenzene (4- 1,4-difluorobenzene 6 Liter (sccm) size Sampling Kits* Sampling Kits*
bromofluorobenzene) 125 hour 0.5–2 0.0008" 24217 $720 24216 $620
In nitrogen, 104 liters @ 1800psig 24 hour 2–4 0.0012" 24160 $720 24165 $620
1ppm cat. # 34408 (ea.) $585 12 hour 4–8 0.0016" 24161 $720 24166 $620
100ppb cat. # 34425 (ea.) $705 8 hour 8–20 0.0020" 24162 $720 24167 $620
3 hour 20–40 0.0030" 24163 $720 24168 $620
1.5 hour 40–80 0.0060" 24164 $720 24169 $620
0.5 hour 80–350 0.0090" 22101 $720 22100 $620
*Air sampling canisters sold separately. Available in 400cc, 1L, 3L, 6L, and 15L volumes.

9
 Organophosphorus Pesticides
Organophosphorus pesticides (OPPs) are commonly used as insecticides, fungicides, and herbicides. Due to their widespread use
however, they have become an environmental concern. We reccommend the Rtx®-OPPesticides2 column for separating
organophosphorus pesticides (OPP). Separation is improved, and analysis time is significantly reduced, compared to other columns.
The extended upper temperature limit of this phase (330°C) allows analysts to bake out high molecular weight contamination typ-
ically associated with pesticide samples. The low bleed column is a perfect match for sensitive detection systems.

Figure 1 Organophosphorus pesticides on an Rtx®-OPPesticides2 column.

1. dichlorvos 15. monocrotophos 29. aspon 42. fensulfothion
2. hexamethylphosphoramide 16. terbufos 30. malathion 43 bolstar
3. mevinphos 17. dimethoate 31. chlorpyrifos 44. carbophenothion
4. trichlorfon 18. dioxathion 32. trichloronate 45. famphur
5. TEPP 19. fonophos 33. parathion-ethyl 46. triphenyl phosphate (SS)
6. demeton-O 20. diazinon 34. fenthion 47. EPN
7. thionazin 21. disulfoton 35. merphos 48. phosmet
8. tributyl phosphate (IS) 22. phosphamidon isomer 36. chlorfenvinphos 49. leptophos
9. ethoprop 23. dichlorofenthion 37. crotoxyphos 50. tri-o-cresyl phosphate
10. naled 24. chlorpyrifos methyl 38. stirofos 51. azinphos-methyl
11. sulfotepp 25. phosphamidon 39. tokuthion 52. azinphos-ethyl
12. phorate 26. parathion-methyl 40. merphos oxone 53. coumaphos
13. dicrotophos 27. ronnel (breakdown product)
14. demeton-S 28. fenitrothion 41. ethion

GC_EV00602
Column: Rtx®-OPPesticides2, 30m, 0.25mm ID, 0.25µm (cat.# 11243) Inj. temp.: 250°C
Sample: US EPA Method 8141A Custom Standard Mix 1µL 100ppm Carrier gas: helium, constant flow
(100ng on column) Flow rate: 1.0mL/min.
Triphenylphosphate Standard (cat.# 32281) Oven temp.: 80°C (hold 0.5 min.) to 140°C @ 20°C/min.
Tributylphosphate Standard (cat.# 32280) to 210°C @ 4°C/min. (hold 1 min.) to
8140/8141 OP Pesticides Calibration Mix A (cat.# 32277) 280°C @ 30°C (hold 5 min.)
8141 OP Pesticides Calibration Mix B (cat.# 32278) Det: MS
Custom Mixes: Call Restek for Information Transfer line temp.: 280°C
Inj.: 1.0µL splitless (hold 0.4 min.), 4mm double Scan range: 35-400amu
gooseneck inlet liner (cat.# 20785) Ionization: EI

Recommended Columns Sample Preparation

Rtx®-OPPesticides2 Columns (fused silica) CarboPrep™ Cartridges
ID df (µm) temp. limits length cat. # price SPE Cartridge Tube Volume, Bed Weight qty. cat# price
0.18mm 0.20 -20 to 310/330°C 20-Meter 11244 $430 CarboPrep™ 90 3mL, 250mg 50-pk. 26091 $105
0.25mm 0.25 -20 to 310/330°C 30-Meter 11243 $490 CarboPrep™ 90 6mL, 500mg 30-pk. 26092 $119
0.32mm 0.32 -20 to 310/330°C 30-Meter 11241 $510
0.53mm 0.50 -20 to 310/330°C 30-Meter 11242 $565 Excellent for Pesticide Residue Cleanup!

did you know?

We can supply all your organophosphate standards—
See our catalog or website for details.

10
 Carbamates by HPLC
Carbamates are widely used insecticides that pose a health risk as endocrine Recommended Columns
disruptors. Our Ultra Carbamate column, in a 50mm length, separates com-
mon carbamates in less than 10 minutes (Figure 1), significantly less than the Ultra Carbamate Columns
time required by traditional C18 columns. In addition to the best column
Physical Characteristics:
choice for the analysis, we offer reference mixes for Method 531 carbamates, a
particle size: 3µm or pH range: 2.5 to 7.5
performance check mix, and the specified internal standard, 4-bromo-3,5- 5µm, spherical temperature limit: 80°C
dimethylphenyl-N-methylcarbamate (BDMC). pore size: 100Å
3µm Column cat. # price
50mm (2.1mm ID) 9177352 $438
Figure 1 Carbamate pesticides on an Ultra Carbamate column. 50mm (4.6mm ID) 9177355 $454
5µm Column cat. # price
Peak List: 250mm (4.6mm ID) 9177575 $438
1. aldicarb sulfone
2. aldicarb sulfoxide *For post-column derivatization / fluorescence detection appli-
3. oxamyl cations for a 4.6mm ID column the total system dead volume,
4. methomyl including the post-column reactor, must be less than 650µL. For
5. 3-hydroxycarbofuran
6. aldicarb standard post-column reactor systems, we recommend a 250 x
7. propoxur 4.6mm, 5µm column. Call Restek technical service for more
8. carbofuran information.
9. carbaryl
10. methiocarb ordering note
11. 4-bromo-3,5-dimethylcarbamate For guard cartridges for these columns, visit our website at
www.restek.com.
Sample:
Inj.: 5µL cat. # 32274 and
cat. # 32273 mixed 50:50
Conc.: 50µg/mL each
Solvent: methanol Analytical Reference Materials
Column: Ultra Carbamate
Cat. #: 9177355 531.1 Carbamate Pesticide Calibration Mixture
Dimensions: 50 x 4.6mm
Particle size: 3µm (10 components)
Pore size: 100Å aldicarb 3-hydroxycarbofuran
aldicarb sulfone methiocarb
Conditions: aldicarb sulfoxide methomyl
Mobile phase: A: 90:10 water:methanol
B: 90:10 methanol: carbaryl (Sevin®) oxamyl
acetonitrile carbofuran propoxur (Baygon®)
Time (min.) %B 100µg/mL each in methanol, 1mL/ampul
0 10 cat. # 32273 (ea.) $41
10 90
Flow: 1.5mL/min.
Temp.: 27°C
Det.: UV @ 220nm 531.2 Carbamate Pesticide Calibration Mixture
(11 components)
aldicarb methiocarb
aldicarb sulfone methomyl
aldicarb sulfoxide 1-naphthol
carbaryl (Sevin®) oxamyl
carbofuran propoxur (Baygon®)
3-hydroxycarbofuran
100µg/mL in acetonitrile, 1mL/ampul
cat. # 32435 (ea.) $46

LC_0225

Internal Standard
4-bromo-3,5-dimethylphenyl-N-methylcarbamate (BDMC)
100µg/mL in methanol, 1mL/ampul
free literature cat. # 32274 (ea.) $23
Simple, Sensitive HPLC/UV Analysis for Paraquat and Diquat
These highly charged quaternary amines are poorly retained on alkyl stationary phases. Using only
531.1 Performance Check Mix
acetonitrile, water, and a solvation-blocking reagent, our separation system alters the interactions
aldicarb sulfoxide 100µg/mL 3-hydroxycarbofuran 2
among analyte, mobile phase, and stationary phase, and promotes solubility of the analytes in the BDMC 10 methiocarb 20
stationary phase. In our system, the detection limit is 6ppb for either herbicide, and the analysis is In methanol, 1mL/ampul
completed in less than 10 minutes. An optimized solid phase extraction cartridge concentrates the cat. # 32275 (ea.) $41
herbicides for the analysis.
Lit. cat. # 580006

11
Polyaromatic Hydrocarbons (PAHs) by HPLC
Most HPLC PAH methods recommend using a C18 column with fluorescence
and/or UV/VIS detection. Our Pinnacle™ II PAH columns have a highly
Recommended Columns
reproducible modified alkyl phase on Restek manufactured silica, specifically
Pinnacle™ II PAH Columns
developed for this application. Figure 1 shows the analysis of 16 target PAHs
Physical Characteristics:
in less than 18 minutes, and Figure 2 shows a separation of 20 target PAHs and
particle size: 5µm, endcap: fully endcapped
related compounds, in less than 6 minutes, using a 5cm column. spherical pH range: 2.5 to 10
pore size: 110Å temperature limit: 80°C
Figure 1 Baseline separation of 16 PAHs in less than 18 minutes 5µm Column cat. # price
on a Pinnacle™ II PAH column. 50 x 2.1mm 9219552 $364
Peak List: Conc. (µg/mL) 50 x 3.2mm 9219553 $364
Sample: 1. naphthalene 100 150 x 3.2mm 9219563 $389
Inj.: 5µL 2. acenaphthylene 100
Solvent: 1:9 methylene chloride:acetonitrile 3. acenaphthene 100
50 x 4.6mm 9219555 $364
4. fluorene 100 150 x 4.6mm 9219565 $389
Column: Pinnacle™ II PAH (Cat. # 9219563) 5. phenanthrene 50 10 x 2.1mm 921950212 $131
150mm x 3.2mm ID 10
6. anthracene 100 10 x 4.0mm 921950210 $131
7. fluoranthene 50
Conditions: 8. pyrene 50 20 x 2.1mm 921950222 $131
Mobile phase: A: water, B: acetonitrile 9. benzo(a)anthracene 50 20 x 4.0mm 921950220 $131
Time (min.) %B 10. chrysene 50
0 40 6 11. benzo(b)fluoranthene 50 ordering note
7 60 12. benzo(k)fluoranthene 50
11 100 For guard cartridges for these columns, visit our website at
13. benzo(a)pyrene 50 www.restek.com.
17.9 100 4 14. dibenzo(a,h)anthracene 50
18 40 5
15. benzo(ghi)perylene 50
Flow: 1.2 mL/min. 16. indeno(1,2,3-cd)pyrene 50
11
Temp.: ambient
9
Det.: UV @ 254nm
Analytical Reference Materials
13
EPA Method 8310 PAH Mixture (18 components)
acenaphthene dibenzo(a,h)anthracene
12 acenaphthylene fluoranthene
anthracene fluorene
7 8
16
benzo(a)anthracene indeno(1,2,3-cd)pyrene
1 benzo(a)pyrene 1-methylnaphthalene
15
2 14 benzo(b)fluoranthene 2-methylnaphthalene
3 benzo(ghi)perylene naphthalene
LC_0303 benzo(k)fluoranthene phenanthrene
chrysene pyrene
6 8 10 12 14 16 18 min.
500µg/mL each in acetonitrile, 1mL/ampul
cat. # 31841 (ea.) $62

Figure 2 Fast, efficient separation of 20 target PAHs and related EPA Method 8310 Quality Control Check
compounds using a 5cm Pinnacle™ II PAH column. (18 components)
Sample: Peak List: acenaphthene 100µg/mL dibenzo(a,h)anthracene 10
Inj.: 5µL 1. naphthalene acenaphthylene 100 fluoranthene 10
Conc.: 5-10ppm each 2. acenaphthylene anthracene 100 fluorene 100
Sample diluent: methylene chloride:acetonitrile (1:9 v/v) 3. 1-methylnaphthalene benzo(a)anthracene 10 indeno(1,2,3-cd)pyrene 10
4. 2-methylnaphthalene benzo(a)pyrene 10 1-methylnaphthalene 100
Column: Pinnacle™ II PAH (Cat. # 9219555) 5. acenaphthene
50mm x 4.6mm ID benzo(b)fluoranthene 10 2-methylnaphthalene 100
6. fluorene benzo(ghi)perylene 10 naphthalene 100
Conditions: 7. phenanthrene benzo(k)fluoranthene 5 phenanthrene 100
Mobile phase: A: water 8. anthracene
9. o-terphenyl
chrysene 10 pyrene 10
B: acetonitrile
Time (min.) %B 10. fluoranthene In acetonitrile, 1mL/ampul
0 50 11. pyrene cat. # 31843 (ea.) $46
1.5 60 12. p-terphenyl
4.0 100 13. benzo(a)anthracene
5.5 100 14. chrysene EPA Method 8310 Surrogate Standard
5.6 50 15. benzo(b)fluoranthene
Flow: 3.0mL/min. decafluorobiphenyl
16. benzo(k)fluoranthene
Temp.: ambient 17. benzo(a)pyrene 1,000µg/mL in acetonitrile, 1mL/ampul
Det.: UV @ 254nm 18. dibenzo(a,h)anthracene cat. # 31842 (ea.) $23
19. benzo(ghi)perylene
20. indeno(1,2,3-cd)pyrene

free literature
Environmental Flyer
HPLC analyses described in this 8-page publication include
LC_0316 carbamates, carbonyls, explosives, paraquat/diquat, phenoxyacid
herbicides, and polyaromatic hydrocarbons.
Lit. cat. # 59741A

12
 Explosives by HPLC
Common methods for quantifying explosives call for reversed phase HPLC
with UV detection, using a primary column and a confirmation column.
Recommended Columns
While cyano phases typically have been used for the confirmation column,
Ultra C18 Columns (USP L1)
resolution of the target explosive compounds is poor. The Pinnacle™ II
Physical Characteristics:
Biphenyl column provides excellent resolution of Method 8330 explosives, as particle size: 3µm or endcap: fully endcapped
shown in Figure 1, and selectivity is markedly different from C18 phases, mak- 5µm, spherical pH range: 2.5 to 7.5
ing the Pinnacle™ II Biphenyl column an ideal confirmation column. If a pore size: 100Å temperature limit: 80°C
cyano phase must be used for confirmation, we recommend a Pinnacle™ II carbon load: 20%
Cyano column. 5µm Column, 4.6mm cat. # price
150mm 9174565 $372
250mm 9174575 $427
Figure 1 An outstanding column pair for explosives analysis.
For superior performance, use an Ultra C18 primary column... Pinnacle™ II Biphenyl Columns (USP L11)
Peak List: Sample: Physical Characteristics:
1. HMX Inj.: 5µL
2. RDX
5 Conc.: 30µg/mL particle size: 5µm, endcap: yes
3. 1,2-dinitrobenzene (SS) (30ppm) each spherical pH range: 2.5 to 7.5
4. 1,3,5-trinitrobenzene Sample diluent: acetonitrile
pore size: 110Å temperature limit: 80°C
5. 1,3-dinitrobenzene Column: Ultra C18
6. tetryl 5µm Column, 4.6mm cat. # price
Cat. #: 9174575
7. nitrobenzene 7 Dimensions: 250 x 4.6mm 150mm 9209565 $360
8. 3,4-dinitrotoluene (IS) 4
13
Particle size: 5µm 250mm 9209575 $412
9. 2,4,6-trinitrotoluene Pore size: 100Å
10. 4-amino-2,6-dinitrotoluene
11. 2-amino-4,6-dinitrotoluene Conditions: ordering note
12. 2,6-dinitrotoluene Mobile phase: water:methanol For guard cartridges for these columns, visit our website at
13. 2,4-dinitrotoluene 3 8 9 (44:56, v/v)
11
Flow: 1.0mL/min. www.restek.com.
14. 2-nitrotoluene
6 Temp.: 30°C
15. 4-nitrotoluene Det.: UV @ 254nm
16. 3-nitrotoluene
2
1
10
12
14
15
16
Analytical Reference Materials
Nitroaromatics and Nitramine
Explosives by HPLC (14 components)
1,3-dinitrobenzene 2-nitrotoluene
LC_0254
2-amino-4,6-dinitrotoluene 3-nitrotoluene
4-amino-2,6-dinitrotoluene 4-nitrotoluene
2,4-dinitrotoluene RDX
0 2 4 6 8 10 12 14 16 18 min.
2,6-dinitrotoluene tetryl
HMX 1,3,5-trinitrobenzene
...coupled with a Pinnacle II™ Biphenyl column. nitrobenzene 2,4,6-trinitrotoluene
1,000µg/mL each in acetonitrile, 1mL/ampul
Sample: cat. # 33905 (ea.) $95
Inj.: 10µL
Conc.: 30µg/mL (30ppm) each
Sample diluent: acetonitrile
Sample temp.: ambient 8095 Internal Standard
Standard: Cat. #: 31452, 31453, 31450, 31451 3,4-dinitrotoluene
1,000µg/mL in methanol, 1mL/ampul
Column: Pinnacle II Biphenyl
™

Cat. #: 9209565 cat. # 31452 (ea.) $23

Dimensions: 150 x 4.6mm
Particle size: 5µm 8330 Surrogate
Pore size: 110Å
1,2-dinitrobenzene
Conditions: 1,000µg/mL in methanol, 1mL/ampul
Mobile phase: water:methanol, 0:50, v/v
Flow: 1.5 mL/min. cat. # 31453 (ea.) $23
Temp.: ambient
Det.: UV @ 254nm
free literature
HPLC Analysis of Trace-Level Explosives Using
Pinnacle II™ C18 and Cyano Columns
Pinnacle II™ C18 reversed phase columns and Pinnacle II™ Cyano
normal phase columns are effective primary and confirmation
columns for analyzing explosives according to US EPA Method
8330A. Analytical conditions and example chromatograms are
presented in this 2-page note. Per recommendation in the
method, the same mobile phase is used for the primary and
confirmation analysis.
LC_0322 Lit. cat. # 59361

13
 Environmental Essentials
Direct Injection Liners - What’s a drilled uniliner? See page 5. O-Rings
ID*/OD & cat.# /price A B
Description Length (mm) ea. 5-pk.
DI Liners for Agilent 5890 & 6890 GCs (For 0.25/0.32/0.53mm ID Columns)
4.0 ID 21054 21055
Drilled Uniliner® ▲ 6.3 OD x 78.5 $64 $253
C D
4.0 ID 21054-214.1 21055-214.5
Siltek® Drilled Uniliner ®▲ 6.3 OD x 78.5 $69 $273
4.0 ID 20756 20771
Drilled Uniliner® ▼ 6.3 OD x 78.5 $64 $284
4.0 ID 20508 20509 E F
Double Gooseneck Drilled Uniliner ®▲ 6.3 OD x 78.5 $64 $253
4.0 ID 20954 20989
Double Gooseneck Drilled Uniliner® ▼ 6.3 OD x 78.5 $64 $284
1.0 ID 21390-214.1 21391-214.5 G H
E N D

Siltek® 1mm Drilled Uniliner® ▲ 6.3 OD x 78.5 $74 $295

DI Liners for Varian 1177 GCs (For 0.25/0.32/0.53mm ID Columns)
4.0 ID 21470 21471
T H I S

Drilled Uniliner® ▲ 6.3 OD x 78.5 $64 $285

I
4.0 ID 21468 21469
Drilled Uniliner® ▼ 6.3 OD x 78.5 $64 $285
I N S T A L L S

DI Liners for Shimadzu 17A, 2010, and 2014 GCs (For 0.32/0.53mm ID Columns)
3.5 ID 21285 21286 Max. temp. qty. cat.# price
Open-top Drilled Uniliner® ▲ 5.0 OD x 95 $69 $274
A) Viton® O-Rings for Agilent GCs
3.5 ID 21287 21288 250°C 25-pk. 20377 $21
Open-top Drilled Uniliner® ▼ 5.0 OD x 95 $69 $274 B) Graphite O-rings for Agilent & Varian split liners (6.35mm ID)
3.5 ID 21289 21290 450°C 10-pk. 20296 $31
5.0 OD x 95 $77 $303 B) Graphite O-rings for Agilent & Varian splitless liners (6.5mm ID)
Gooseneck Drilled Uniliner® ▲
C O L U M N

450°C 10-pk. 20298 $31

3.5 ID 21291 21292
C) 5mm Graphite Liner Seals for Varian 1078/1079 GCs
Gooseneck Drilled Uniliner® ▼ 5.0 OD x 95 $77 $303
450°C 10-pk. 22683 $34
DI Liners for PerkinElmer GCs (For 0.32/0.53mm ID Columns) D) Viton ® O-Rings for Shimadzu 17A, 2010, and 2014 GCs
4.0 ID 20819 20822 250°C 10-pk. 21477 $15
Auto SYS™ Drilled Uniliner® ▲ 6.2 OD x 92.1 $64 $253 E) Graphite O-Rings for Shimadzu 17A, 2010, & 2014 Split Liners
450°C 5-pk. 20243 $46
4.0 ID 21293 21294
E) Graphite O-Rings for Shimadzu 17A, 2010, & 2014 Splitless Liners
Auto SYS™ Drilled Uniliner® ▼ 6.2 OD x 92.1 $64 $253
450°C 5-pk. 20244 $46
4.0 ID 21295 21296 F) Silicone O-Rings for PerkinElmer Auto SYS™ GCs
Auto SYS™ Gooseneck Drilled Uniliner® ▲ 6.2 OD x 92.1 $78 $312
250°C 10-pk. 20262 $7.50
4.0 ID 21297 21298 G) Viton® O-Rings for PerkinElmer PSS
Auto SYS™ Gooseneck Drilled Uniliner® ▼ 6.2 OD x 92.1 $79 $312 250°C 10-pk. 20366 $10
Direct Injection Liners for Thermo Electron TRACE™ & Focus SSL (0.32 & 0.53mm ID columns) H) Inlet Liner Seals for TRACE™ PTV
450°C 2-pk. 21392 $28
5.0 ID 22411 22412
I) Graphite Sealing Ring for TRACE™ and Focus SSL Instruments
Drilled Uniliner® ▲ 8.0 OD x 105 $75 $295
450°C ea. 21898 $17
5.0 ID 22413 22414 I) Graphite Sealing Rings for TRACE™ and Focus SSL Instruments
Drilled Uniliner® ▼ 8.0 OD x 105 $75 $295 450°C 2-pk. 21899 $27.50
▲ ▼
*Nominal ID at syringe needle expulsion point. Hole on top. Hole on bottom.

did you know?

We can supply all your sample extract clean-up needs.
See our catalog or website for details.

14
Restek Septa
• Precision molding assures consistent, accurate fit.
• Ready to use.
• Do not adhere to hot metal surfaces.
• Packaged in non-contaminating glass jars.
Septum Diameter
Thermolite® Septa
25-pk. /price 50-pk./price 100-pk./price
HANDY
5mm (3/16") 27120 $42 27121 $62 27122 $103
Thermolite® Septa septum size chart
6mm (1/4") 27123 $42 27124 $62 27125 $103
•Usable to 340°C inlet
7mm 27126 $42 27127 $62 27128 $103 Septum
temperature. Diameter
8mm 27129 $42 27130 $62 27131 $103
Instrument (mm)
9mm 27132 $42 27133 $62 27134 $103 •Excellent puncturability. Agilent (HP)
9.5mm (3/8") 27135 $42 27136 $62 27137 $103 5880A, 5890, 6890,
10mm 27138 $42 27139 $62 27140 $103 6850, PTV 11
11mm (7/16") 27141 $42 27142 $62 27143 $103 5700, 5880 9.5/10
11.5mm 27144 $42 27145 $62 27146 $103 On-Column Injection 5
12.5mm (1/2") 27147 $42 27148 $62 27149 $103 IceBlue™ Septa Thermo Electron
17mm 27150 $47 27151 $82 27152 $158 •Usable to 250°C inlet TRACE™ GC 17
Shimadzu Plug 27153 $42 27154 $62 27155 $103 temperature. GCQ w/TRACE™, PTV 17
8000 series 17
IceBlue™ Septa •General-purpose septa. Finnigan (TMQ)
9mm 27156 $37 27157 $67 GC 9001 9.5
•Excellent puncturability.
9.5mm (3/8") 27158 $37 27159 $67 GCQ 9.5
10mm 27160 $37 27161 $67 •Ideal for SPME. QCQ ™
9.5
11mm (7/16") 27162 $37 27163 $67 TRACE™ 2000 9.5
11.5mm 27164 $37 27165 $67 Gow-Mac
12.5mm (1/2") 27166 $37 27167 $67 6890 series 11
17mm 27168 $38 27169 $71 All other models 9.5
Shimadzu Plug 27170 $38 27171 $71 PerkinElmer
Sigma series 11
BTO® Septa BTO® Septa 900,990 11
5mm CenterGuide™ 27100 $65 27101 $115 •CenterGuide™ design— 8000 series 11
6mm (1/4") 27102 $65 27103 $115 requires less force for initial Auto SYS™ 11
9mm CenterGuide™ 27104 $65 27105 $115 penetration. Auto SYS™ XL 11
9.5mm (3/8") 27106 $65 27107 $115 Pye/Unicam
•Usable to 400°C inlet
10mm 27108 $65 27109 $115 All models 7
temperature.
11mm (7/16") CenterGuide™ 27110 $65 27111 $115 Shimadzu
11.5mm CenterGuide™ 27112 $65 27113 $115 •Each batch GC-FID tested. All models Plug
12.5mm (1/2") CenterGuide™ 27114 $65 27115 $115 SRI
•Bleed and temperature opti- All models Plug
17mm CenterGuide™ 27116 $85 27117 $170 mized; ideal for demanding Tracor
Shimadzu Plug 27118 $85 27119 $170 GC and GC/MS applications. 540 11.5
550,560 9.5
220,222 12.5
Varian
Dual Vespel® Ring Inlet Seals - Eliminates the need for a washer!
Injector type:
0.8mm ID Dual Vespel® Ring Inlet Seal 2-pk. /price 10-pk./price Packed column 9.5/10
Siltek® Treated 21242 $58 21243 $264 Split/splitless
Gold-Plated 21240 $58 21241 $264 1078/1079 10/11
Stainless Steel 21238 $45 21239 $195 1177 9
1075/1077 11
1.2mm ID Dual Vespel ® Ring Inlet Seal 2-pk. /price 10-pk./price
Siltek® Treated 21248 $58 21249 $264
Gold-Plated 21246 $58 21247 $264
Stainless Steel 21244 $45 21245 $195
septum
handling tips
Replacement Inlet Seals with Washers •Handle septa carefully, to
Single-Column Installation, 0.8mm 0.25/0.32mm ID Dual-Column 0.53mm ID Dual-Column prevent contamination.
Opening* Installation, 1.2mm Opening Installation (1/16-inch opening) •Minimize bleed—use
2-pk./price 10-pk./price 2-pk./price 10-pk. /price 2-pk./price 10-pk./price preconditioned, low-bleed
Stainless Steel Inlet Seal septa.
21315 $45.25 21316 $195.70 20390 $45 20391 $195 20392 $45 20393 $195 •Follow septum and
Gold-Plated Inlet Seal instrument manufacturers’
21317 $58.75 21318 $264.25 21305 $58.75 21306 $264.25 — — recommendations.
Siltek® Treated Inlet Seal
21319 $58.75 21320 $264.25 21307 $58.75 21308 $264.25 — —
*0.8mm ID stainless steel inlet seal is similar to Agilent part #18740-20880,
0.8mm ID gold-plated inlet seal is similar to Agilent part #18740-20885.
Restek Trademarks:
CarboPrep, Crossbond, IceBlue, MegaMix, MXT, Pinnacle, Press-Tight, Rtx, Rxi, SeCure, SilcoCan, Silcosteel, Siltek, Sulfinert, Thermolite, TO-Can, Uniliner.

Other Trademarks:
BTO (Chromatography Research Supplies, Inc.), Freon, Vespel, Viton (E.I. du Pont de Nemours & Co., Inc.), QCQ (Finnigan Corp.), SUMMA (Moletrics), Auto SYS (Perkin-Elmer),
Baygon (S.C. Johnson & Son, Inc.), TRACE (Thermo Scientific), Sevin (Union Carbide Corp.), Veriflo (Veriflo Corp.)

Lit. Cat.# 580127

© 2007 Restek Corporation.
Biodiesel Solutions
Innovative Products for Simple,
Reliable Biodiesel Analysis

• MXT®, Rtx®, and Stabilwax® biodiesel columns—

engineered specifically for high performance
biodiesel analysis.
• GC accessories to simplify your lab work and
increase productivity.
• Analytical reference materials—high quality
standards for reliable results.

Integrated retention gaps—

The Ultimate
Biodiesel Solution!
See page 5 for details

Chromatography Products
www.restek.com 800-356-1688 • 814-353-1300
Introduction to Biodiesel Analyzing Total Glycerin in Biodiesel
Today, as oil prices climb and pollution levels soar, Rtx®-Biodiesel TG Fused Silica Columns
there is significant worldwide interest in alternative Glycerin in biodiesel falls out of solution, causing gumming in fuel systems and
fuels. Biodiesel is one of the most popular alterna- malfunctioning of engine parts, which eventually leads to inferior engine per-
tive fuels available today. It may be used in engines, formance. Total glycerin presents itself in two forms: free glycerin and bound
either pure or blended with diesel fuel, to reduce glycerin in the form of glycerides. Derivatization is required for analysis, and
exhaust pollutants. It can be produced easily from both ASTM D6584 and EN 14105 use N-methyl-N-trimethylsilytrifluoroac-
sunflowers, soy, rapeseed, tallow, lard, yellow grease, etamide derivatization reagent.
and other sources. Chemically, it is the product
obtained when a vegetable oil or animal fat is react- A 10m x 0.32mm ID Rtx®-Biodiesel TG column with a 2m x 0.53mm ID reten-
ed with an alcohol in the presence of a catalyst, such tion gap is ideal for glycerin analysis. The retention gap is factory coupled using
as sodium or potassium hydroxide, to produce fatty Restek’s unique Alumaseal™ connector (Figure 1). This innovative connector is
acid methyl esters. leak-tight and low dead volume, making it advantageous for high temperature
work. The data in Figure 2 show the elution of glycerin, monoglycerides, diglyc-
Methods used to test the quality of biodiesel fuels erides, and triglycerides in B100 biodiesel following ASTM Method D6584, uti-
can be categorized into three types based on the tar- lizing cool on-column injection. The Rtx®-Biodiesel TG column provides good
get compounds: ASTM D6584 and EN 14105 test for resolution and signal-to-noise ratios for mono-, di-, and triglycerides.
total glycerin, EN 14103 tests for fatty acid methyl
esters (FAMEs), and EN 14110 tests for residual
methanol. These methods may be performed using
either fused silica or metal columns, but the column Figure 1: The Alumaseal™ connector
chosen must have extremely high temperature toler- The Alumaseal™ connector is the best column connector for coupling fused silica and metal
ance. Restek offers both fused silica and metal columns, even columns of different internal diameters. Made of aluminum, it is designed for
columns designed specifically for high temperature high temperature performance. These connectors have been factory-coupled and tested using
biodiesel analysis. These columns, the Rtx®- temperature programmed mass spectrometry and have shown no signs of leaks, even at 430°C.
Biodiesel TG, MXT®-Biodiesel TG, Stabilwax®, and The Alumaseal™ connector offers:
Rtx-1® column lines, offer outstanding performance •A leak-tight connection.
for biodiesel testing. •Low dead volume.

Rtx®-Biodiesel TG Columns (fused silica) •Low thermal mass.

Rtx®-Biodiesel TG Columns: •High inertness.
• Low column bleed at high temperatures.
• Alumaseal™ connector provides leak-free con-
nection, retention gap extends column life.
• Complete resolution for all compounds from Figure 2 The Rtx®-Biodiesel TG column meets resolution criteria
interference peaks. and shows excellent response for determining glycerin in biodiesel.
Description temp. limits cat.# price
10m, 0.32mm ID, 0.10 to 330/380°C 10292 $250
10m, 0.32mm ID, 0.10 w/2m x
0.53mm retention gap** to 330/380°C 10291 $295
15m, 0.32mm ID, 0.10 to 330/380°C 10294 $305
15m, 0.32mm ID, 0.10 w/2m x tricaprin (IS)
0.53mm retention gap** to 330/380°C 10293 $365
**Connected with low-dead-volume Alumaseal™ connector.
monoglycerides

Biodiesel Calibration Standards butanetriol (IS) diglycerides

Concentration is µg/mL in pyridine. Volume is 1mL/ampul unless
glycerin triglycerides
otherwise noted.
Compound Solvent cat.# price
(s)-(-)-1,2,4-butanetriol 1,000 33024 $33
(s)-(-)-1,2,4-butanetriol (5mL) 1,000 33032 $113 GC_PC00890
diolein(1,3-di[cis-octadecenoyl] glycerol) 5,000 33022 $31
glycerin 500 33020 $31
monolein
(1-mono[cis-9-octadecenoyl]-rac-glycerol) 5,000 33021 $31 0 10 20
monopalmitin 5,000 33026 $33
tricaprin (1,2,3-tricaprinoyl glycerol) 8,000 33025 $33 Column: Rtx -Biodiesel TG, 10m, 0.32mm ID, 0.10µm connected to 2m x 0.53mm
®

tricaprin (1,2,3-tricaprinoylglycerol) (5mL) 8,000 33033 $113 Hydroguard™ tubing using Alumaseal™ connector (cat.# 10291)
triolein (1,2,3-Tri[cis-octadecenoyl] glycerol) 5,000 33023 $31 Sample: biodiesel (B100) plus monoolein, diolein, triolein, glycerin, butanetriol, tricaprin
Inj.: 1µL, cool on-column
Inj. temp.: oven track
Silylation Derivatization Reagents Carrier gas: hydrogen, constant flow
Flow rate: 4mL/min.
Compound CAS# cat.# price Oven temp.: 50°C (hold 1 min.) to 180°C @ 15°C/min. (hold 7 min.) to
MSTFA (N-methyl-N-trimethylsilytrifluoroacetamide) 230°C @ 30°C/min. to 380°C @ 30°C/min. (hold 5 min.)
Det.: FID
10-pk. (10x1g) 24589-78-4 35600 $65 Det. temp.: 380°C
25g Flex Tube 24589-78-4 35601 $75

2 www.restek.com • 800-356-1688
Comparing Fused Silica to Metal Figure 3 Fused silica columns, labeled as stable up to 430°C, show
High temperature applications shorten the life- significant pitting and breakdown.
time of fused silica columns due to deterioration
of the polyimide resin used to make the columns.
When fused silica columns are exposed to oven
temperatures over 400°C the polyimide coating
becomes brittle and the deactivation of the col-
umn is compromised. Figure 3 shows the effect of
cycling a commercially available fused silica col-
umn to 430°C for 5 minutes 100 times. Although
the column was labeled as stable up to 430°C, the
polyimide coating shows damage. The inertness of
the column also deteriorates as shown by the loss
of peak symmetry for the internal standard
butanetriol over multiple injections (Figure 4).
Metal MXT®-Biodiesel TG columns are a better
alternative to fused silica columns. As shown in
Figure 4, they clearly outperform high tempera- Before
ture fused silica columns under the cycling condi-
tions required for biodiesel analysis. Metal MXT®-
Biodiesel TG columns offer greater stability and
longer column lifetimes compared
to fused silica columns.

After

100 temperature cycles to 430°C totaling 500 minutes at

maximum temperature.

Figure 4 Stable peak shape for internal standard butanetriol on

MXT®-Biodiesel TG columns gives more accurate quantification.

2
Asymmetry value

1.8 MXT® tubing is

1.6
more stable than
HT Fused Silica
fused silica!
1.4

1.2 MXT-Biodiesel TG

0.8
1 8 15 22 29 36 43 50 57 64 71 78 85 92 99 100
Number of Injections

800-356-1688 • www.restek.com 3
Metal Column Solutions: Two Options for Increased Stability and Performance
• 0.32mm MXT®-Biodiesel TG column with a 0.53mm retention gap,
factory coupled with an Alumaseal™ connector
• 0.53mm MXT®-Biodiesel TG column with a built-in 0.53mm
Integra-Gap™ integrated retention gap

The primary advantage of using metal MXT® columns is that they are more stable at high temperatures than fused silica columns.
This means they will exhibit lower bleed, improving analytical performance, and have longer lifetimes, making them a cost-effective
option. They also can be brought to high temperatures (430°C) allowing nonvolatile material to be baked off of the column, remov-
ing carryover contamination and improving cycle times.
Metal MXT®-Biodiesel TG columns are offered in the same column dimensions as their fused silica counterparts. Two different col-
umn configurations are available for cool on-column injection: 1) a 10m (or 15m) x 0.32mm ID MXT®-Biodiesel TG column fac-
tory coupled to a 2m x 0.53mm retention gap using an Alumaseal™ connector, and 2) a 14m x 0.53mm ID MXT ®-Biodiesel TG col-
umn with a built-in 2m x 0.53mm ID Integra-Gap™ integrated retention gap.
Target analytes resolve well and the solvent and triglyceride peaks show excellent symmetry on both columns (Figures 5 and 6), but
the 0.53mm MXT ®-Biodiesel TG column with the Integra-Gap™ integrated retention gap eliminates the need for a connector, mak-
ing connector-related leaks a thing of the past. Peak shape for butanetriol is very good, demonstrating inertness, and the resolution
and response for the mono-, di- and triglycerides is excellent. The leak-proof 0.53mm MXT®-Biodiesel TG column with the Integra-
Gap™ integrated retention gap is the ultimate biodiesel solution (Figure 7).

Figure 5 Derivatized B100 samples resolve well on the 15m x 0.32mm MXT®-Biodiesel TG column, which is factory
coupled to a 0.53mm retention gap using an Alumaseal™ connector.

Monoglycerides Monoglycerides Diglycerides Triglycerides

Column: MXT®-Biodiesel TG, 15m, 0.32mm ID, 0.10µm (cat.# 70291) with
a 2m x 0.53mm MXT® retention gap connected with an
tricaprine (IS)

Alumaseal™ connector (17m total length)

Sample: biodiesel (B100), derivatized
Inj.: cool on-column injection
1µL in heptane
Inj. temp.: oven track
Glycerin Carrier gas: hydrogen, constant flow
Flow rate: 3mL/min.
Oven temp.: 50°C (hold 1 min.) to 180°C @ 15°C/min. to 230°C @ 7°C/min. to 380°C @
30°C/min. (hold 5 min.)
butanetrial (IS)

Det.: FID @ 380°C

GC_PC00968

0 10 20
Time (min)
 Figure 6 Excellent chromatographic quality and resolution on the 0.53mm MXT®-Biodiesel TG column, with the
Integra-Gap™ integrated retention gap.

Monoglycerides Monoglycerides Diglycerides Triglycerides

The best solution for

analyzing total glycerin
in biodiesel!

tricaprine (IS) Column: MXT®-Biodiesel TG, 14m, 0.53mm ID, 0.16µm (cat.# 70289) with
a 2m x 0.53mm Integra-Gap™ retention gap
(16m total length)
Sample: biodiesel (B100), derivatized
Inj.: cool on-column injection
1µL in heptane
Glycerin Inj. temp.: oven track
butanetrial (IS)

Carrier gas: hydrogen, constant flow

Flow rate: 4mL/min.
Oven temp.: 50°C (hold 1 min.) to 180°C @ 15°C/min. to 230°C @ 7°C/min. to
380°C @ 30°C/min. (hold 5 min.)
Det.: FID 380°C

GC_PC00969

0 10 20
Time (min)

Figure 7 The Ultimate Biodiesel Solution: MXT®-Biodiesel TG

column with Integra-Gap™ integrated retention gap. Get More!
The 0.53mm MXT -Biodiesel TG columns are an innovative alternative to using a 0.32mm col-
®

umn coupled to a 0.53mm retention gap. Restek applied the Integra-Gap™ integrated retention
Biodiesel Related
gap technology to the 0.53mm Articles Online
MXT®-Biodiesel TG columns, elimi-
nating the column coupling. These “Biodiesel Analysis by
100% leak-proof columns feature
a built-in retention gap, reducing European Methodology”
the risk of peak broadening and
tailing, and guaranteeing the user Retention Gap
many analyses without downtime. “Analyze Biodiesel
Oil for Glycerin”
www.restek.com/biodiesel
MXT®-Biodiesel TG Columns
• Fast analysis times and sharp glyceride peaks.
• Stable at 430°C for reliable, consistent performance.
• Integra-Gap™ built-in retention gap eliminates manual connection.

MXT®-Biodiesel TG Columns (Siltek® treated stainless steel)

Description temp. limits cat.# price
14m, 0.53mm ID, 0.16 w/2m Integra-Gap™ -60 to 380/430°C 70289 $530
10m, 0.32mm ID, 0.10 -60 to 380/430°C 70292 $325
10m, 0.32mm ID, 0.10 w/2m x 0.53mm retention gap** -60 to 380/430°C 70290 $480
15m, 0.32mm ID, 0.10 -60 to 380/430°C 70293 $325
15m, 0.32mm ID, 0.10 w/2m x 0.53mm retention gap** -60 to 380/430°C 70291 $480

*Total column length=16 meters.

**Connected with low-dead-volume Alumaseal™ connector. 800-356-1688 • www.restek.com 5
Analyzing FAMES in Biodiesel Analyzing Methanol in Biodiesel
FAMEs are the desired end product of biodiesel production and they are ana- Methanol is commonly used to produce biodiesel
lyzed to determine the percent of usable fuel in the final product. A Stabilwax® by derivatizing the fatty acids to methyl esters. The
fused silica GC column affords excellent peak symmetry, resolution, and amount of residual methanol must be determined
reproducibility for determining the FAMEs and linolenic acid methyl ester because engine performance can be negatively
content in B100 biodiesel fuel, following European standard method EN affected if the methanol concentration in the final
14103. product is too high. Methanol in biodiesel is quan-
tified using a headspace method (e.g. EN 14110).
As shown in Figure 8, C14:0-C24:1 FAMEs and linolenic acid methyl ester can We recommend an Rtx®-1 column (30m, 0.32mm
be determined in less than 11 minutes using a 30m x 0.32mm ID x 0.25µm ID, 3µm) for this analysis. The selectivity of the
Stabilwax® column. Particularly notable are the stability of the baseline, excel- Rtx®-1 column is ideal for resolving methanol
lent peak symmetry, and baseline resolution of all compounds of interest. The from interfering peaks in biodiesel fuels.
Stabilwax® column shows excellent peak shape for all FAMEs, even at low
concentrations, which is critical for accurate quantification (Table 1).

Figure 8 Stable baselines, excellent peak symmetry, and rapid, Conclusion

baseline resolution of all compounds characterize FAMEs Whether testing for glycerin, FAMEs, or methanol,
analyses on a Stabilwax® column. Restek can supply the high quality chromatogra-
phy products required for biodiesel testing. We
offer an array of metal and fused silica GC
Rapeseed FAMEs on Stabilwax®
1. myristic acid C14:0 7. linolenic acid C18:3 columns designed for high performance biodiesel
2. palmitic acid C16:0 8. arachidic acid C20:0 analysis, including our innovative MXT®-
3. palmitoleic acid C16:1 9. gadoleic acid C20:1
IS methyl heptadecanoate 10. behenic acid C22:0
Biodiesel TG column with an Integra-Gap™ inte-
4. stearic acid C18:0 11. erucic acid C22:1 grated retention gap (Table II). Our columns,
5. oleic acid C18:1 12. lignoceric acid C24:0 accessories, and analytical reference materials are
6. linoleic acid C18:2 13. nervonic acid C24:1
designed to improve analytical quality, simplify lab
work, and increase productivity. Rely on Restek for
innovative solutions to your biodiesel testing
needs.
GC_PC00917

Column: Stabilwax®, 30m, 0.32mm ID, 0.25µm (cat.# 10624) Rtx®-1 Columns (fused silica)
Sample: rapeseed source of biodiesel (B100), prepared according to European Method EN 14103
Inj.: 1.0µL split (split ratio 100:1), Cyclosplitter® inlet liner (cat.# 20706) (Crossbond® 100% dimethyl polysiloxane)
Inj. temp.: 250°C ID df (µm) temp. limits length cat. # price
Carrier gas: hydrogen, constant flow, 3mL/min. 0.32mm 3.00 -60 to 280/300°C 30-Meter 10184 $465
Linear velocity: 60cm/sec.
Oven temp.: 210°C (hold 5 min.) to 230°C @ 20°C/min. (hold 5 min.)
Det.: FID
Det. temp.: 250°C

Table I Sources of FAMEs in B100 biodiesel fuel (% m/m).

Soy Tallow Rapeseed Yellow Grease
Myristic acid C14:0 0.21 1.7 0.11 0.68
Palmitic acid C16:0 11.24 25.5 4.1 16.35
Palmitoleic acid C16:1 0.2 3.27 0.27 1.23
Stearic acid C18:0 4.04 14.41 1.8 9.32
Oleic acid C18:1 21.93 40.34 58.57 47.8
Linoleic acid C18:2 53.84 12.02 22.2 20.01
Linolenic acid C18:3 7.29 0.99 13.26 2.93
Arachidic acid C20:0 0.36 0.4 0.79 0.46
Gadoleic acid C20:1 0.26 1.03 1.79 0.39
Behenic acid C22:0 0.45 0.57 0.44
Erucic acid C22:1 0.13 0.23
Lignoceric acid C24:0 0.16 0.34 0.3 0.24
Nervonic acid C24:1 0.17 0.54

Stabilwax® Column (fused silica)

(Crossbond® Carbowax® polyethylene glycol)
ID df (µm) temp. limits length cat. # price
0.32mm 0.25 40 to 250°C 30-Meter 10624 $460

www.restek.com • 800-356-1688
 ASTM D6584
Table II GC Column Selection Guide for Biodiesel Fuel Methods. EN 4103 EN 14105
Free and total
EN 14110

Ester and glycerine and

Fused Silica Free and Total Linoleic acid mono, di, and
GC Columns Description Injection Type Glycerin methyl esters triglycerides Methanol
Rtx-Biodiesel TG 15m, 0.32mm ID, 0.1µm w/ 2m x
(max temp. 380°C) 0.53mm ID retention gap cool on-column 10293 — 10293 —
Rtx-Biodiesel TG
(max temp. 380°C) 15m, 0.32mm ID, 0.1µm PTV** 10294 — 10294 —
Rtx-Biodiesel TG 10m, 0.32mm ID, 0.1µm w/ 2m x
(max temp. 380°C) 0.53mm ID retention gap cool on-column 10291 — 10291 —
Rtx-Biodiesel TG
(max temp. 380°C) 10m, 0.32mm ID, 0.1µm PTV** 10292 — 10292 —

Stabilwax 30m, 0.32mm ID, 0.25µm split/splitless — 10624 — —

Rtx-1 30m, 0.32mm ID, 3.0µm headspace — — — 10184

Metal (MXT)
GC Columns
*MXT-Biodiesel TG 14m, 0.53mm ID, 0.16µm w/ 2m
(max temp. 430°C) Integra Gap cool on-column 70289 — 70289 —
MXT-Biodiesel TG 15m, 0.32mm ID, 0.1µm w/ 2m x
(max temp. 430°C) 0.53mm ID retention gap cool on-column 70291 — 70291 —
MXT-Biodiesel TG
(max temp. 430°C) 15m, 0.32mm ID, 0.1µm PTV** 70293 — 70293 —
MXT-Biodiesel TG 10m, 0.32mm ID, 0.1µm w/ 2m x
(max temp. 430°C) 0.53mm ID retention gap cool on-column 70290 — 70290 —
MXT-Biodiesel TG
(max temp. 430°C) 10m, 0.32mm ID, 0.1µm PTV** 70292 — 70292 —
*Recommended for total glycerin analysis.
**PTV=programmed temperature vaporizer.

GC Accessories
Thermolite® Septa
• Usable to 340°C inlet temperature.
• Preconditioned and precision molded.
• Do not adhere to hot metal surfaces.
• Packaged in precleaned glass jars.

Septum Diameter 25-pk./price 50-pk./price 100-pk. /price

9mm 27132 $42 27133 $62 27134 $103
9.5mm (3/8") 27135 $42 27136 $62 27137 $103
10mm 27138 $42 27139 $62 27140 $103
11mm (7/16") 27141 $42 27142 $62 27143 $103
11.5mm 27144 $42 27145 $62 27146 $103
12.5mm (1/2") 27147 $42 27148 $62 27149 $103
17mm 27150 $47 27151 $82 27152 $158
Shimadzu Plug 27153 $42 27154 $62 27155 $103

Parker Balston® Hydrogen Generators

• Proton Exchange Membrane (PEM) cell eliminates the need for liquid electrolytes.
• Reliably generate 99.9995% pure hydrogen, for better chromatography.
• Cost-effective, convenient, and safe alternative to high pressure cylinders.
Specifications
Purity: 99.9995% pure hydrogen Physical Dimensions: 17.12"h x 13.46"w x 17.95"d
Delivery Pressure: 10-100psig ± 1psig (69-689kPa ± 7kPa) (43.48 x 34.19 x 45.6cm)
1
Outlet Port: /8" compression Shipping Weight: 40 lbs. (18kg) dry
Electrical Requirements: 100-230VAC/50-60Hz
• Dimensions: 17.12" x
Description Capacity qty. cat.# price 13.46" x 17.95"
H2PEM-100 100cc/min. ea. 23065 $5248 • 40 lb. dry weight
H2PEM-165 165cc/min. ea. 23066 $6753
H2PEM-260 260cc/min. ea. 23067 $8661
H2PEM-510 510cc/min. ea. 23068 800-356-1688
$11,288 • www.restek.com 7
 Restek Electronic Leak Detector Leak Detector Facts
• Reliable thermal conductivity leak detector. Detectable gases: helium, nitrogen, argon, carbon dioxide
Battery: Rechargeable Ni-MH, 7.2 volt
• Responds to leaks in less than 2 seconds. Operating
• Audible alarm plus LED readout. Temperature Range: 32°-120°F (0°-48°C)
• Auto zeros with the touch of a button. Humidity Range: 0-97%
• Built-in rechargeable 7.2-volt battery. CE Approved: Yes

Description qty. cat.# price

Small, compact Leak Detector with 110Volt Battery Charger ea. 22451 $839
Leak Detector with 220Volt European Battery Charger ea. 22451-EUR $839
unit—easy to hold
Leak Detector with 220Volt UK Battery Charger ea. 22451-UK $839
and operate.
Caution: The Restek Electronic Leak Detector is NOT designed for determining leaks of combustible gases. A combustible gas detector should be used
for determining combustible gas leaks under any condition. The Restek Electronic Leak Detector may be used for determining trace amounts of hydrogen
in a GC environment only.

Capillary Ferrules—For 1/16-Inch Compression-Type Fittings

Graphite Ferrules Vespel®/Graphite Ferrules
• Preconditioned to eliminate out-gassing. • 60%/40% Vespel®/graphite blend, offering the
• High-purity, high-density graphite. best combination of sealing and workability.
• Stable to 450°C. • Stable to 400°C.
Also available in
Ferrule ID Fits Column ID qty. Graphite Vespel®/Graphite
money-saving
0.5mm 0.32mm 10-pk. 20201 $30 20212 $36
50-packs! 0.8mm 0.45/0.53mm 10-pk. 20202 $30 20213 $36

tech tip
Which FID Jet Should I Use?
Replacement Jets
There are two FID jet • Available untreated or Siltek® treated, for maximum inertness.
configurations for Agilent GCs.
Capillary Adaptable FID Replacement Jet for Agilent 5890/6890/6850 GCs
The longer “adaptable” jet fits
both 5890 and 6890 GCs, and 0.011-Inch ID Tip Similar to Agilent part # qty. cat.# price qty. cat.# price
can be used with capillary or Standard 19244-80560 ea. 20670 $55 3-pk. 20671 $148
packed columns. The shorter High-Performance Siltek® Treated 19244-80560 ea. 20672 $62 3-pk. 20673 $178
“dedicated” jet is for the FID
in the 6890 GC that is Capillary Dedicated FID Replacement Jet for Agilent 6890/6850 GCs
designed only for use with 0.011-Inch ID Similar to Agilent part # qty. cat.# price qty. cat.# price
capillary columns. Standard G1531-80560 ea. 21621 $44 3-pk. 21682 $130
High-Performance Siltek® Treated G1531-80560 ea. 21620 $49 3-pk. 21683 $145
Restek Trademarks:
Alumaseal, Crossbond,
Cyclosplitter, Integra-Gap,
MXT, Stabilwax, Thermolite, FID Jet Removal Tool for Agilent 5890/6890/6850 FIDs
Rtx, Restek logo, Siltek. • Securely grips jet in socket for easy removal or installation.
• Unique, ergonomic handle—easy to hold.
Other Trademarks:
Balston (Parker Intangibles Description qty. cat.# price
LLC), Vespel (E. I. du Pont de
FID Jet Removal Tool for Agilent 5890/6890/6850 FIDs ea. 22328 $39
Nemours & Co., Inc.)

Restek Corporation Presorted Standard

110 Benner Circle US Postage
Bellefonte, PA 16823-8812 PAID
Restek

Lit. Cat.# 580207

© 2007 Restek Corporation.