Frequently Asked Question (FAQ)

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While other companies can pyrolyze samples at the same temperature as the Frontier pyrolyzer, why don’t they guarantee the reproducibility of pyrograms?
We think that other companies do not guarantee the reproducibility in the specifications in the manual mode, because their reproducibilities of pyrograms are generally 20-30%, and its reliability is too poor to put it in the specifications.
Frontier Lab has developed a high precision temperature controller, with extensive optimization of relevant parts used, we thus are able to guarantee the reproducibility be less than 2% relative standard deviation by peek area ratios for trimer of polystyrene pyrolyzed at 550°C and internal standard (methyl stearate).
How do we know the pyrolyzer that we are currently using is working properly?
The pyrogram of polystyrene is used to monitor system performance. A polystyrene standard (P/N: PY1-4908) is included with each pyrolyzer. The standard includes 5% methyl stearate (5%). Analyze the standard and compare the pyrogram to the one shown in Chapter 8, Fig. 8.2 (Guarantee of basic performance) of the operation manual.
What is the rate of pyrolysis? How does it compare with Currie Point Pyrolyzers? How would the influences reflect in the final results?
The time it takes to heat the sample to 600⁰ in N2 using a vertical furnace is less than 100msec, as reported by Dr. Tsuge, Emeritus Professor of Nagoya University. Theoretically, the time will be reduced by one seventh in a helium atmosphere, and is, therefore, comparable to the rate achieved when using a Currie point foil. The actual rate of pyrolysis, the reproducibility and stability of the furnace temperature and the physicality (e.g. weight, density, distribution of the sample in the furnace, etc.) determine the reproducibility of the pyrogram. These factors also play a role in what pyrolzates are formed as well as their relative intensities.
In the case of Currie point devices, the temperature of the ferromagnetic foil increases instantly; however, the contact between the sample and sample holder is different in each run, which reduces the reproducibility of the pyrograms. In the case of pyrolyzers using a filament, the sample position in the quartz sample tube (id. 2 mm or less, length 30 mm) relative to the filament coils differs in each run, resulting in poor reproducibility.
What is the precision of the temperature control?
The furnace temperature is within +/- 0.1°C of the set point for Frontier’s Multi-Shot Pyrolyzer.
Does any adsorption occur in the pyrolyzer?
The pyrolysis tube is quartz, and the inner surface of the interface needle, which is located between the GC injection port and the pyrolyzer furnace, is deactivated with our Ultra ALLOY® technology, thus adsorption inside the pyrolyzer should be negligible. All pyrolyzers must meet stringent inertness specifications. Inertness of the entire GC system (i.e., from the pyrolyzer liner to the outlet of the separation column). The operator must also consider the possibility of system contamination when using the pyrolyzer. For example, if too much sample is placed in the sample cup the pyrolysis tube could be contaminated. Frontier recommends that a system check sample be analyzed daily. Over time the series of pyrograms will enable the operator to quickly ascertain system performance and determine when routine maintenance is necessary.
What is the purpose of the cooling gas used with the pyrolyzer? Is it required?
Cooling gas is required when using a Frontier multi-mode (a.k.a. Double Shot) pyrolyzer. The gas reduces the time required to cool the furnace temperature down to the initial temperature when using methods that require the temperature of the furnace to be cycled. On the other hand, a Single-Shot Pyrolyzer is used at a constant temperature and cooling gas is not required.
How much cooling gas is needed for the Multi-Shot Pyrolyzer? What grade of gas do you recommend? What is the actual cooling time?
The consumption of cooling gas is 7L/min at an inlet supply pressure of 500kPa. Compressed air with a mist-trap or industry grade compressed air or N2 can be used.
The EGA/PY-3030D pyrolyzer takes about 5 minutes to cool from 600 to 100°C.
The PY-2020iD pyrolyzer takes about 20 minutes to cycle from 600 to 100°C.
What is the difference in the final results between evolved gas analysis using the Pyrolyzer and a head-space sampler?
Because the pyrolyzer is designed to minimize cold spots in its flow path from the furnace to the GC injection port, a wide range of compounds from low boiling to high boiling compounds up to C40 compounds can be analyzed. The amount of sample required is several tens of milligrams; therefore, chemical species at as low as several ppb can be analyzed.
Although, head space samplers can handle several hundreds mg of samples, the thermal desorption of target compounds hidden inside the sample matrix is difficult. Because headspace sampling is normally limited to 200°C and the fact that most have a relatively long flow path from the sample heater to GC injection port, compounds analyzed by headspace sampler is generally limited to relatively low boiling compounds, up to C20.
There are three types of pyrolyzers; filament, Currie point, and heating furnace pyrolyzers. What are the differences?
The basic difference is how the sample is heated.
Filament type: the sample is held in a quartz tube (id 2mm) that is placed in a filament coil. The filament is rapidly heated and the sample is heated by radiant heat from the filament. The “set point’ pyrolysis temperature, however, is often different from the actual sample temperature.
Currie point type: the sample is wrapped in a ferromagnetic sample holder (pyrofoil). The foil is heated by electromagnetic induction. The sample is heated by thermal radiation. The temperature attained depends on the composition of the ferromagnetic foil.
Heating furnace type: the sample is placed in a small, inert sample cup and dropped into a preheated furnace. The sample is instantly heated to the set-point temperature of the furnace.
How does dead volume (un-swept areas of the sample flow path.) influence the data?
The flow path from the quartz pyrolysis tube to the GC injection port is designed so that dead volumes are minimized. During “final checkout”, we confirm that there is no peak broadening due to the presence of dead volume. A simple way to check for “dead” volume is to change the flow through the system while holding the column flow constant. The peak width at half height should be independent of the inlet flow, assuming the column flow is held constant. Contamination will have the appearance of ‘dead’ volume and it is much more likely to occur than the the sudden appearance of ‘dead’ volume.
Can we buy pyrolyzer furnace and controller separately?
Our pyrolyzer is marketed as an integrated package consisting of the heating furnace and the temperature controller. We therefore do not sell heating furnace or temperature controller separately.
When the sampler is removed from the pyrolyzer, will air get into the pyrolyzer? Does it cause any trouble?
The sampler on the top of the pyrolyzer is being purged with carrier gas at all times. When air gets into the system it is purged out of the system in a minute or two. For example, when the total carrier gas flow rate is 50 mL/min, any air in the system will be completely purged two minutes after the sampler is re-attached.
What is Single-Shot-GC analysis?
The sample cup is dropped into the preheated pyrolysis furnace, causing the sample to be instantly pyrolyzed. Pyrolyzates flow through the needle interface and into the GC injector. Sample vapors are split, a small portion of the pyrolyzates flow into a GC separation column for analysis (PY-GC). This technique is generally called, Flash Pyrolysis.
What is evolved gas analysis (EGA)?
The EGA technique is a simple thermal analysis technique, in which relatively volatile gases released by the continuous programmed heating of a sample are directly analyzed by GC/MS. The technique uses a deactivated metal tube (Ultra ALLOY, 0.15 mm id., 2.5 m in length) to connect the split/splitless injection port and the MS detector. The EGA thermograms obtained from this technique provide a wide range of information including details about additives, volatile components contained in sample, and decomposition temperature of the sample.
What is the Double-Shot-GC analysis?
This technique allows a polymer sample to be sequentially analyzed for volatile and polymer components. Volatile components contained in a sample are first desorbed at relatively low temperatures, this is followed by flash pyrolysis in which the sample polymer is dropped into the furnace heated at high temperatures and the base polymer is pyrolyzed.
What is heart-cut EGA-GC analysis?
This is an analytical technique in which only the evolved gases from a selected temperature zone of an EGA thermogram are introduced into a GC separation column for analysis. This is useful for the analysis of composite materials.
When doing “manual” analysis, how do I retrieve the sample cup from the pyrolyzer furnace?
To recover a sample cup when using an Eco-Stick SF, remove the sampler and use the sample cup retriever (Eco-Pickup) supplied as a standard accessory.
When using an Eco-Stick LF, remove the sampler, then pull the Eco-Stick out using tweezers.
Is it all right to turn off the temperature controller immediately after the analysis?
Turning off the power to the temperature controller also turns off the cooling fan that cools the sample cup positioned at the top of the quartz pyrolysis tube. If the cooling fan stops, the temperature of the top seal on the quartz liner increases due to thermal conduction, and radiant heat from the hot pyrolysis furnace. Frontier recommends that the temperature controller be turned off only when the temperature of the pyrolysis furnace is >300°C.
How do I clean the quartz pyrolysis tube?
First remove the quartz pyrolysis tube from the furnace – refer to the video on the frontier web site for details. Polymeric residues and tars are removed by heating the quartz tube with a propane torch. Alternatively, heat the tube in an electric muffle furnace. Inorganic contaminants may be removed by acid treatment. If this is done, heat the quartz tube to “red” hot before using it.
How often should I clean the quartz pyrolysis tube?
Contamination of the pyrolysis tube is linked to the type and amount of sample being analyzed as well as the number of injections.. When ghost peaks are observed in the chromatograms or pyrograms, or the peak response is low due to adsorption on the tube surface, the quartz pyrolysis tube and/or interface needle must be cleaned or replaced.
Can I use MS as a detector in evolved gas analysis with air as a carrier gas?
MS can be used as a detector when air is used as the carrier gas, but note the followings:
1. GC oven temperature should be 200ºC or below. If it is higher, the inertness of EGA capillary tube (P/N: UADTM-2.5N) can be damaged.
2. This may cause some damage to the MS filament and shorten the life. The degree of damage depends on the filament thickness and oxidation resistance. Please check with the manufacturer of the MS. Use of quasi-air that is helium mixed with several percent of oxygen can extend the filament life.
3. FID detector poses no problems.
4. Customer takes all responsibilities to any damage caused by this.
When pyrolyzer is not used, should the carrier gas remain on?
There is no need to keep the carrier gas flow on.
If the pyrolyzer is not going to be used for a long time, does the furnace temperature need to be lowered?
We recommend that the furnace temperature be maintained at 200°C when not in use. This prevents the seals from contracting or expanding with changes in the working environment. This helps to maintain seal integrity.
Can I easily remove the pyrolyzer from a GC and install it on another GC?
This will be a very simple process. When moving the pyrolyzer to a different GC, we recommend that mounting brackets be installed on each GC in order to facilitate easy installation of the pyrolyzer.
Can a liquid sample be analyzed while pyrolyzer is installed on GC?
When analyzing a liquid sample, you can use a liquid sampler which is provided as a standard accessory. Inject sample using a normal micro syringe. The furnace of the pyrolyzer serves as injection port; therefore; set the furnace temperature 50°C higher than the GC injector. Better reproducibility will be obtained than is normally obtained by direct injections to the GC injector.
How do I remove the quartz pyrolysis tube?
Remove the pyrolyzer from the GC injection port, and loosen the sampler base nuts at the top of the pyrolyzer. Then loosen the interface union located at the bottom of the pyrolyzer. Now the quartz tube can easily be pulled out. See Operation Manual for details.
Does the pyrolyzer come with a control PC?
No. The pyrolyzer control software is downloaded to the PC used to control the GC or GC/MS.
What are the required specifications for the control PC?
A hard disk space of 10MB is required. See this page for supported OS. Any PC used for GC or GC/MS control should be adequate. The Pyrolyzer requires a USB port for their communication interface.
Is control software included with the pyrolyzer?
Yes. The control software comes standard with the pyrolyzer.
Does the pyrolyzer control software depend on the control software for the GC/MS?
The control software for Pyrolyzer is independent from that for GC/MS. However, “READY” and “START” signals from GC or GC/MS are shared with the pyrolyzer control software.
What is the difference between Multi-Shot Pyrolyzer and Double-Shot Pyrolyzer (old model)?
The major difference is the method used to heat the furnace. The Double-Shot pyrolyzer uses a cartridge heater (max temp. 800ºC) while the Multi-Shot Pyrolyzer uses a smaller ceramic heater (max temp. 1050ºC). Using the ceramic heater reduces the cycle time of the furnace. It heats faster and it cools faster that an old style cartridge heater/metal block. The rate is three-times faster than that of the old style. See EGA/PY-3030D catalog for details.
Can I upgrade my Single-Shot Pyrolyzer (PY-3030S) to Multi-Shot Pyrolyzer (EGA/PY-3030D)?
Upgrading to a Multi-Shot Pyrolyzer is not possible.
The sampler (Double-Shot or Single-Shot) will no longer hold the sample cup stick. Can it be fixed?
This is caused by wear of the chuck that holds the sample cup stick. It needs to be sent to us for repair, or you can purchase the chuck from us and fix it by yourself. Call your local dealer or contact us directly.
Double-Shot sampler does not slide well. Would cleaning help?
The double shot sampler must be disassembled and a special lubricant must be applied on the sliding surface; therefore, it must be sent to us for repair. Check with your local dealer or contact us directly.
Is regular inspection of the Pyrolyzer needed?
Yes. Please consult the Pyrolyzer Operation Manual to see what regular maintenance is recommended. This is a good time to perform regular maintenance of your GC (injection port liner, seals, septum, etc.) for the best performance of the system.
Are yearly maintenance contracts available?
Yes. Call your local distributor (see listing on our website) or contact us using the website.
We would like to conduct evolved gas analysis (EGA). What other accessories do we need in addition to Pyrolyzer?
None. The Double-Shot Pyrolyzer or Multi-Shot Pyrolyzer is all that is needed to perform EGA.
When fluorocarbon polymer is pyrolyzed, hydrogen fluoride (HF) is formed. Can the acid give adverse effects to the separation column?
The amount of HF formed by the pyrolysis of a sample quantity (about 0.2 mg) of fluorocarbon polymer is very limited. Our experience showed that there is almost no impact to the separation column. If you would not like to introduce the HF gas to the column, a piece of quartz wool dampened with 10% aqueous solution of potassium hydroxide (KOH), followed by drying, is placed at the bottom of the glass insert in the GC injector (immediately before the separation column) will prevent the HF gas from being introduced to the column. This will trap the HF gas. However, please note that other acids are trapped here and therefore will not be analyzed.