Leading the way in material characterization“On-line micro reaction sampler”
The on-line micro reaction sampler is a device that allows a small amount of a sample and reagent to react under semisupercritical or supercritical fluid conditions in a small glass capsule (id 2 mm, length 30-35 mm), and is fitted to a MultiFunctional Pyrolyzer, then reaction products formed are analyzed online directly by GC.

Features• Reactions under high pressure and high temperature
in a closed system

10

Supercriticalfluid conditions

8MPa *Polyamides that can hardly be analyzed by normal reactive pyrolysis GC or PyGC can be analyzed by organic alkali derivatization under high pressures andhigh temperatures.

• Online GC analysis of reaction products
After reaction in a sealed glass capsule, the products can be analyzed online
directly by introducing them to a GC separation column without working up thereaction mixture.

• High pressure reactions using a small amount ofsample and reagent

5 µL
643 µL

21 µL

Methanol

0100

200
300
400
Temperature (ºC)
*1 MPa = 10 atm

Temperature and pressure isothermals
with varied volumes of methanol

Only a few milligrams of sample and reagent are required for the online micro
reaction sampler; therefore, it is safe to handle.
The figure on the right shows the calculated relationship between the pressure and temperature inside of a glass capsule, when 1, 3 and 5 µL of methanol
are added to the glass capsule (volume: 76 µL). Methanol becomes a supercritical fluid above the critical temperature and critical pressure (T=239ºC,
P=8.1 MPa). A supercritical fluid has unique properties and often gives quite different results from those of normal conditions.

Typical applications of the micro reaction sampler
Reactive pyrolysis of nylon 6.6

Reactive pyrolysis of fat (butter)

Polyamide (e.g. nylon) is one of the polymers that are difficult
to analyze using ordinary reactive pyrolysis GC or Py-GC.
However, performing the analysis at elevated pressuressignificantly enhances the organic alkali hydrolysis andderivatization process.
The figure below shows the chromatograms of nylon 6.6
obtained by 1) flash pyrolysis, 2) conventional reactive
pyrolysis, and 3) reactive pyrolysis at elevated pressure.
Only the chromatogram 3) has large peaks which areindicative of the nylon 6.6 structure.

Methyl esterification of vegetable oils and animal fats which
are the common sources of biodiesel fuel can be studied
using the micro reaction sampler.

GC: 40→320ºC (20 ºC/min)
Column: UA5-30M-0.25F

1) Flash pyrolysis
Py: 600ºC, Eco-Cup

The top chromatogram was obtained using conventional
reactive pyrolysis (350ºC). The bottom chromatogram wasobtained using the micro reaction sampler. While the ratiosof the methyl esters of the aliphatic acids are comparable,
the ratios of methylated glycerol are quite different.

1) Reactive pyrolysis in open system

GC: 40→320ºC (20 ºC/min)
Column: UA5-30M-0.25F
Py: 350ºC, Eco-Cup
Reagent: tetramethylammonium hydroxide (TMAH), 5 µL

Hexamethylenediamine
C16C18’Glycerol567891011C1412 min

C18Squalene

C18’’

C28

dimethyl- trimethyl-2) Conventional reactive pyrolysis
Py: 300ºC, Eco-cup
Reagent: tetramethylammonium hydroxide (TMAH), 5 µL

C103C6C845C12C24 C26C20 C2267891011121314151617 min

1617 min2) Reactive pyrolysis using the micro reaction sampler
56789101112 min3) Reactive pyrolysis using the micro reaction sampler
Py: 300ºC, reaction time: 1 hr
Reagent: TMAH, 5 µL

Py: 100ºC, reaction time: 1 hr
Reagent: TMAH, 5 µL

Glyceroldimethyl-Dimethyl adipate

trimethyl-Tetramethyl
hexamethylenediamine

56789101112 min

3456789101112131415

Operating principal
The operating sequence described earlier is shown below:
Cross-section of the On-line microreaction sampler

On-line micro reaction sampler and glass capsulebefore and after crushing

Rotating knob

BeforeAfter
Crushing rod
Slides up and down

Sampler baseHe
Expanded view

Reactionchamber

30-35 mm

Sealed glasscapsule

Sample and reagent sealed
in glass capsule
Four side-openings forflushing the reaction
products.

Pyrolysis tube

Using on-line micro reaction sampler(1) Place sample and reagent in a glass capsule.
(2) Insert the glass capsule into the capsule holder until ithits the bottom of the hole. The capsule holder and thebase must be chilled in a freezer in advance.

(1)

(2)

(3)

(4)

Crushing rod

(5)

HeHe

(3) Flame-seal the top end of the capsule using a small
torch as in the figure on the right.

(4) Place the sealed capsule in the reaction chamber andReagent
attach it to the sampler. Attach the sampler to theO-ringMulti-Functional pyrolyzer, purge the air from the Glass
sampler. When the furnace and GC are READY, push Capsule
Capsulethe sampler down into the furnace. The sample isholder
allowed to react at a given temperature for a given
Sample andBase
period of time. Alternatively, batch treatment can be reagent
done outside of the sampler such as in an oven.

Torch(5) After the reaction is completed, rotate the top knob tolower the crushing rod. When the capsule shatters, thereaction products are flushed onto the GC column.

Specifications
Compatible pyrolyzer : EGA/PY-3030D, PY-3030S
Glass capsule: od. 2.5 mm, length 25~34 mm
Max use temperature : 400ºC
Max reagent volume : 10 µL

GC INJ

Contents in package• On-line Micro Reaction Sampler• Standard accessories
Glass capsule sealing assembly( incl. O-ring S3)
Glass capsule BSampler standReaction chamber (spare)O-ring S4 (spare)1SUS pyrolysis tube 3030

Qty

P/N

1 pc

PY1-1050

1 pc
3 pc
1 set (40 pcs)
1 pc
1 pc
5 pcs
2 pc

PY1-5315
PY1-5319
PY1-5113
UV1-3802
PY1-5311
UV1-7701
PY1-3321* On-line Micro Reaction Sampler (P/N: PY1-1050) contains all the items listed above.
The quantities of each parts may differ from the package when ordering individually.

4-16-20 Saikon, Koriyama, Japan, 963-8862
TEL:81(24)935-5100 FAX:81(24)935-5102
www.frontier-lab.com
For product improvement, appearance and specifications are subject to change without notice.

V220208