MARKES U LTR A User Manual

Series 2

ULTRA

Thermal Desorption
Autosampler

Multi-function TD autosampler with optional
reading/writing of electronic tube tags

Series 2

ULTRA

1. Patent# GB 2395785 (Automated re-collection using a single TD autosampler), 2. Patent# US 6,446,515 B2, 3. Patent# GB 2337513 US 6,564656 B1

4. Patent# GB 2336649

Thermal desorption technology

Thermal desorption (TD) is a highly versatile, sensitive
and labour-saving sample preparation technique for the
measurement of volatile and semi-volatile organic
compounds (VOC and SVOC) in air and materials. It is
applicable to GC-compatible organics ranging in
volatility from acetylene to n-C40and a few inorganic
gases; including nitrous oxide, SF6, CS2and H2S. Key
applications include:

• Environmental and workplace air monitoring

• Civil defence and forensic analysis

• Materials and materials emissions testing

• Food, flavour and fragrance profiling

Many material samples such as drugs, foods, textiles,
polymers, paints, etc. can be directly thermally
desorbed by weighing them into empty TD sample
tubes.

Alternatively, vapours in gas or air can be concentrated
on- or off-line onto sorbent tubes/traps before TD­GC(MS) analysis.

ULTRA 2 Main Features

• Adds 100-tube automation to any UNITY or UNITY 2 TD platform to increase productivity.

• TubeTAG™: Reading/writing of RFID tags on sorbent tubes is now fully integrated with automated TD
operation. This revolutionizes tube and sample traceability.

• Stringent sample sealing, before and after desorption. Patented DiffLok™ caps preserve sample and blank­tube integrity and ensure compliance with standard methods.

• Quantitative sample re-collection (SecureTD-Q) is offered as standard on every series 2 U

LTRA-UNITY

system for repeat analysis of critical samples and/or method validation.

• Automation of SecureTD-Q av

ailable using single or double U

LTRA configurations; totally tag-compatible for

fail-safe tracking of which sample was re-collected onto which tube.

• State-of-the-art TD analytical performance. U

LTRA 2 simply adds automatic tube processing to the

peerless thermal desorption analytical performance of UNITY 2.

• U

LTRA-reliability – field-proven,

mechanically-simple automation ensures robust operation.

• Method compliance – incorporates the ambient temperature/no-flow leak test of UNITY 2 as a guarantee of
data integrity. Option of internal standard addition to blank or sampled tubes as a further aid to analytical
quality assurance.

• Optional dry-purging of sorbent tubes (in the sampling direction) as part of the automated sequence. This
minimizes water interference and is recommended by standard methods.

• Innovative, compact design – minimizes bench space.

Innovation and excellence in
thermal desorption

Since 1997 Markes International has re-engineered
analytical thermal desorption for the 21st century.
Harnessing unparalleled technical expertise, the
company has developed a suite of ‘universal’ TD
systems and unique sampling accessories incorporating
key proprietary innovations such as:

• SecureTD-Q™ for repeat analysis and automated
re-collection using a single TD autosampler

• RFID tube tagging (TubeTAG™)

• Diffusion-locking for effective tube sealing and
robust automation

• Innovative low volume valving specifically
designed for TD

Many of these innovations now set the standard for TD
instrumentation worldwide.

3

4

2

1

Series 2 ULTRA

ULTRA 2 is an innovative, robust and method-compliant
thermal desorption (TD) autosampler for up to a
hundred industry standard (3.5-inch) sample tubes,
featuring the option of integrated reading/writing of
RFID tube tags. It adds to any series 1 or series 2
UNITY TD platform to provide unmatched TD-GC(MS)
analytical performance and extended unattended
operation e.g. through an entire weekend.

Method-compliant automation

Series 2 ULTRA adds to any UNITY or UNITY 2 platform
desorber to offer unattended thermal desorption of up
to 100 capped tubes. The slimline design consists of
ten horizontal trays each containing up to ten tagged
or untagged tubes. Each tube in turn is loaded into
the analytical position and sealed into the carrier gas
flow path. The following analytical steps then all take
place on the U

LTRA 2 autosampler:

• Ambient temperature/no flow leak testing

• Optional dry purging and/or internal standard

addition

• Pre-purge of air from the tube

• Primary (tube) desorption

As vapours desorb from the primary sample tube in
U

LTRA 2 they are swept through the short, inert, heated

link line into the electrically­cooled focusing trap of UNITY
(2) in a stream of carrier gas.
All subsequent stages of
thermal desorption (trap purge,
trap desorption, triggering of
the GC(MS) run, etc.) take
place on UNITY (2) in the
normal way.

Uncompromised TD analytical
performance

Series 2 ULTRA automates UNITY 2 without
compromising its peerless analytical performance. The
combined system provides a universal TD platform for
up to 100 3.5-inch tubes offering simultaneous
analysis of volatiles & semi-volatiles, quantitative
recovery of high boilers (including n-C40) and the
option of low flow path temperatures for compatibility
with labile analytes such as mercaptans. Systems offer
splitless capillary operation for trace level work and
single or double split methods for high concentration
samples such as stack emissions and residual solvent
in materials.

Series 2 U

LTRA-UNITY systems maintain all the

analytical advantages of UNITY 2 (as described in the
associated brochure) and offer the following additional
benefits relating to the automatic processing of TD
sample tubes.

Clean indoor air pumped onto multi-sorbent tube and analysed by TD-GCMS

1,1-difluoroethane

Ethanol

Isopentane

1,1-difluoro-1-chloroethane

Dichlorodifluoromethane

1,1,1,2-tetrafluoroethane

Hexane

Acetone

Freon 113

Propanol

Trichlorofluoromethane

Dichloromethane

Methylcyclohexane

Benzene

Tetrachloromethane

Ethyl acetate

Hexanal

Toluene

Ethyl benzene

Ethylcyclohexane

o/p xylene

Tetrachloroethane

α-pinene

Trimethylbenzene

Decane

Styrene

Limonene

Undecane

Benzyl alcohol

Nonanal

Dodecane

Tridecane

Tetradecane

DiffLok™ caps seal tubes

No analyte losses from Tenax tubes capped with DiffLok

caps and analysed on U

LTRA over a 24 hr period

Toluene

Benzene

Time loaded tube spent on ULTRA prior to desorption (mins)

Peak area counts (x10

6

)

Xylene

effectively & simplify TD

automation

100-Tube automation optimizes
productivity

ULTRA 2 maximises the throughput and revenue
generation potential of your TD-GC(MS) system. It
offers capacity for up to 100 sample tubes together
with overlap mode. Sample overlap means that
desorption of a subsequent tube can begin while
GC(MS) analysis of a previous sample continues – thus
minimizing analytical cycle times.

With typical GC(MS) cycle times of 40 minutes, your
series 2 U
unattended processing of 100 tubes over a standard
60-hour weekend; this represents significant revenue
potential with minimal labour costs.

LTRA-UNITY TD-GC(MS) system offers

Patented tube sealing
mechanism

Tubes on series 2 ULTRA autosamplers are sealed with
Markes’ unique patented DiffLok caps. DiffLok caps
simply push on to both ends of every tube and
preserve sample integrity by preventing both analyte
loss and artifact ingress. Even volatile analytes are
confidently preserved on sorbent tubes giving identical
recovery for standards at the beginning and end of a
100-tube sequence. DiffLok caps have been field
proven to seal sampled and blank tubes much more
effectively than older push on cap designs (Ref 1).

Ref 1: Diffusive Monitor Issue 9 (Nov 1997), Losses
from ATD-400 by P. P. Ballesta

Schematic of DiffLok cap

Sample tube

pushes into cap

Inert or stainless steel outer body

(shown transparent)

here

Highly efficient tube sealing

Coned end for

Auto-alignment with

tube nozzle on ULTRA 2

(the TD autosampler)

O-ring for sealing

Threaded diffusion-locking insert

plain, cylindrical body

tube into cap

in