Separated Determination of Carbon Black in Chloroprene ...
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Nobuaki Okubo Separated Determination of Separated Determination of Carbon Black in Chloroprene Rubber Carbon Black in Chloroprene Rubber by by Simulation of Heating Rate Conversion Simulation of Heating Rate Conversion
Transcript of Separated Determination of Carbon Black in Chloroprene ...
Nobuaki Okubo
Separated Determination of Separated Determination of Carbon Black in Chloroprene Rubber Carbon Black in Chloroprene Rubber
bybySimulation of Heating Rate ConversionSimulation of Heating Rate Conversion
Simulation of Heating Rate Conversion
Low heating rate measurements
CRTA (Control-Rate Thermal Analysis)
Simulation of Heating Rate Conversion
< Conventional method >
Temperature Temperature
ΔW
ΔW
Simulation of Heating Rate Conversion
Arrhenius Plot for Multiple Reactions
1 / T
ℓog
B
Reaction X Reaction Y
Low Heating Rate
Certain Heating Rate
ΔE = Slope × R
Simulation of Heating Rate Conversion
Algorithm for Simulation of Heating Rate Conversion
DTG peak detection
Output
Peak overlapping N
Peak separation ΔE calculation
ΔE calculation (each peak)
Time - Temperature conversion
Date integration
Y
DTG curve
Peak separation
Time-Temp. Conversion
1000
800
600
400
200
0
0
-20.0
-40.0
-60.0
-80.0
-100.0
TG Measurement Results of Chloroprene RubberSample : SRF70 (CB 37.4wt%)
0.0 1.0 2.0 3.0 4.0Time / hrs
Tem
pera
ture
/ ºC
TG /
%
Measurements Results
Temperature
TG
N2 Air
Carbonaceous-residue
Added CB
Volatile-matter content andHydrocarbon content Rubber Content
Added Carbon Black
Materials
20.130SRF30
29.650SRF50
37.470SRF70
FT50
SRF10
HAF50
SAF50
Sample #
29.650150FT
7.810
65SRF
29.65030HAF
29.65018SAF
CB content(wt%)
CompoundingRatio (phr)
Particle size(nm)
CarbonBlack
Chloroprene Rubber Samples
Materials
20.130SRF30
29.650SRF50
37.470SRF70
FT50
SRF10
HAF50
SAF50
Sample #
29.650150FT
7.810
65SRF
29.65030HAF
29.65018SAF
CB content(wt%)
CompoundingRatio (phr)
Particle size(nm)
CarbonBlack
Chloroprene Rubber Samples
Materials
7.810SRF10
20.130SRF30
29.65065SRFSRF50
37.470SRF70
FT50
HAF50
SAF50
Sample #
29.650150FT
29.65030HAF
29.65018SAF
CB content(wt%)
CompoundingRatio (phr)
Particle size(nm)
CarbonBlack
Chloroprene Rubber Samples
Measurements
InstrumentsTG/DTA6200 Thermogravimetry/Differential Thermal Analyzer
0.01～100ºC/min
0.03µV/0.06µV
0.1µg/0.2µg
±200mg
Horizontal Differential Type
RT ～ 1100ºC
Scanning Rate
DTA RMS Noise/Sensitivity
TG RMS Noise/Sensitivity
TG Range
Balance System
Temperature Range
Measurements
Measurement conditionSample weigh : 5mgSample pan : Pt open panPurge gas flow Rate : 200ml/minTemperature program :
R.T.
800 ºC 800 ºC
20 ºC/min 2 ºC/min
N2 Air
Time
200 ºC
2.00
1.50
1.00
0.50
0.00
TG and DTG Curves for added CB in Chloroprene RubberSample : SRF70 (CB 37.4wt%)
300.0 400.0 500.0 600.0Temperature / ºC
DTG
/ %
/ºC
Measurements Results
TG /
%
-20.0
-40.0
-60.0
-80.0
-100.0
DTG
TG
41.7%37.9%
Added CB: 37.4%
2.00
1.50
1.00
0.50
0.00
TG and DTG Curves for added CB in Chloroprene RubberSample : SRF10(7.8wt%), SRF30(20.1wt%), SRF50(29.6wt%) and SRF70(37.4wt%)
Temperature / ºC
DTG
/ %
/ºC
TG /
%
-20.0
-40.0
-60.0
-80.0
-100.0
300.0 400.0 500.0 600.0
TG
DTG
Compound ratio dependence
Compound ratio dependence
37.941.737.4SRF70
30.032.529.6SRF50
21.022.220.1SRF30
7.37.17.8SRF10
Simulation Method0.1ºC/min (wt%)
Conventional Method2ºC/min (wt%)
Added CB(wt%)Sample
Quantitative results of the added CB with four different compound ratios
2.00
1.50
1.00
0.50
0.00
TG and DTG Curves for added CB in Chloroprene RubberSample : SAF50 (CB 29.6wt%, Particle size 18nm)
Temperature / ºC
DTG
/ %
/ºC
TG /
%
-20.0
-40.0
-60.0
-80.0
-100.0
300.0 400.0 500.0 600.0
TG
DTG
Particle size dependence
17.5%30.3%
Particle size dependence
29.830.929.6FT50
30.032.529.6SRF50
29.533.929.6HAF50
30.317.529.6SAF50
Simulation Method0.1ºC/min (wt%)
Conventional Method2ºC/min (wt%)
Added CB(wt%)Sample
Quantitative results of the added CB with four kinds of particle size
• Effective to the separation of the consecutive weight changes.• Much less measurement time compared to the low heating measurement
and CRTA- Applicative to the measured data.
• Higher accuracy in the quantitative analysis of CB in rubbers compared tothe conventional method.
Simulation of Heating Rate Conversion ;
Thus Simulation of Heating Rate Conversion method enables the higher accuracy the quantitative analysis without lowering measurement efficiency.This method is effective for the quantitative analysis of CB in
rubbers.
Summary
