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Journal of Thermal Analysis and Calorimetry

, Volume 133, Issue 1, pp 649–657 | Cite as

Discuss the heat release capacity of polymer derived from microscale combustion calorimeter

  • Qiang Xu
  • Cong Jin
  • Andrea Majlingova
  • Agoston Restas
Article
  • 215 Downloads

Abstract

Heat release capacity is known as a combination of the thermal stability and combustion properties, which can be used to classify the flammability of materials. It can be derived from microscale combustion calorimeter test results or from additive molar group contributions. PMMA and two kinds of extruded polystyrene were tests by microscale combustion calorimeter with 9 heating rates. Heat release capacity was calculated for the tested materials by 5 algorithms from the literatures. Adaptability of these 5 algorithms was evaluated in this paper.

Keywords

Heat release capacity Flammability Heating rate Microscale combustion calorimeter Limited oxygen index 

Introduction

Pyrolysis mechanism and related modeling research are based on microscale thermal analysis, and different algorithms are adopted to help evaluating the flammability of materials [1]. Microscale combustion calorimeter (MCC) has been used as microscale test facility to measure the flammability of material with milligram specimen mass in the range of 0.5–50 mg. MCC was developed by the Federal Aviation Administration (FAA) to offer industry a research tool to assist the FAA in its mandate to dramatically improve the fire safety of aircraft materials [2]. The tester is becoming a mainstay in research laboratories due to its ability to obtain meaningful test data. The instrument has been validated by a national consensus organization ASTM International and is now the subject of an ASTM standards publication, designated D7309; the latest version is ASTM D7309-13 [3]. MCC provides a wealth of information on the fire hazard of a material [2] including heat release rate (HRR) per unit mass, heat release capacity η c, and total heat release. η c is defined as the average amount of heat released by combustion of the pyrolysis gases per degree of the temperature rise over the pyrolysis interval [3, 4]. More and more researchers have used MCC in their flame retarded research and flammability evaluation recently [5, 6, 7, 8]. The methodology of using MCC was also studied [9].

In ASTM D7309-13 [3], in section 5 “Significance and Use,” subsection 5.7 mentions “the heat release capacity (η c) is a flammability parameter measured in ‘Method A’ that is unique to this test method,” while in section 6 “Limitations”, subsection 6.1 points out that “the heat release capacity (η c) is independent of the form, mass, and heating rate of the specimen as long as the specimen temperature is uniform at all times during the test.” Note 2 in Sect. 7 “Apparatus” emphasizes “in this test, the heat release capacity (η c) is independent of the test parameters as it is a material property and not a response of a material to a particular set of conditions. Thus, changing the test condition (within certain constraints) will have no effect on the test result.” ASTM D7309-13 provides the calculation of heat release capacity η c (J g−1 K−1) as follows:
$$ \eta_{c} = \frac{{q_{ \hbox{max} } }}{\beta } $$
(1)
where q max = the maximum value of specific HRR q(t) per unit mass in the test, W g−1. β = average heating rate over the measurement range, K s−1.

ASTM D7309-13 also provides η c of 14 commercial plastics obtained by MCC in its annex, but no heating rate is specified.

In a presentation of Lyon RE, and Walters RN, η c was described as [10].
  1. 1.

    A rate-independent flammability parameter.

     
  2. 2.

    An intensive quantity (independent of sample mass).

     
  3. 3.

    Measurable by different laboratory techniques.

     
  4. 4.

    A good predictor of fire and flammability behavior.

     
  5. 5.

    Calculable from chemical structure.

     
  6. 6.

    A material property: dynamic combustion potential.

     
η c is also known as a combination of the thermal stability and combustion properties, each of which is known to be calculable from additive molar group contributions [11]. η c appears to be a true material property that is rooted in the chemical structure of the polymer and is calculable from additive molar group contributions [11]. The rate-independent η c is obtained as [11, 12]
$$ \eta_{\text{c}} = \frac{E}{{\beta m_{0} }}\Delta {\dot{\text{O}}}_{2}^{ \hbox{max} } = \frac{{h_{\text{c}}^{0} \left( {1 - \mu } \right)E_{\text{a}} }}{{eRT_{\text{p}}^{2} }} $$
(2)
where m 0 is initial specimen mass, E = 13.1 ± 0.6 k J g−1 of O2, \( \Delta {\dot{\text{O}}}_{2}^{ \hbox{max} } \) is the maximum mass consumption rate of oxygen, \( h_{\text{c}}^{0} \) is the heat of complete combustion of the pyrolysis gases, μ is the weight fraction of the solid residue after pyrolysis or burning, E a is the global activation energy for the single-step mass loss process or pyrolysis, e is the natural number (2.718), R is the gas constant (8.314 J mol−1 K−1), T p is the temperature at the peak mass loss rate. Equation 2 shows η c to be a particular function of the thermal stability and combustion properties, each of which is known to be calculable from additive molar group contributions. Consequently, η c itself is a material property and should be calculable from the same (or similar) molar groups as the component properties as long as there are no interactions between the chemical structural units [11].
In a FAA report “Thermal Analysis of Polymer Flammability” [4], η c is also described as the average amount of heat released by combustion of the pyrolysis gases per degree of temperature rise over the pyrolysis interval; see Eq. 3. η c is defined at a specific heating rate β 0, but it can be calculated from the data obtained at a different heating rate β using Eq. 4 [4]
$$ \eta_{\text{c}} = \frac{{h_{\text{c}}^{0} }}{{\Delta T_{{{\text{p}},0}} }} $$
(3)
$$ \eta_{\text{c}} = \frac{{q_{ \hbox{max} } }}{\beta }\left[ {\frac{\beta }{{\beta_{0} }}} \right]^{\text{a}} $$
(4)
where a = 2RT max,0/E a, β 0 is a reference heating rate, T max,0 = T max(β 0) is the temperature at maximum pyrolysis, ΔT p,0 = eRT max,0 2 /E a.
In another FAA document “Principles and Practice of Microscale Combustion Calorimetry” [13], η c can also be calculated by
$$ \eta_{\text{c}} = \frac{{h_{\text{c}}^{0} }}{{e^{\gamma } RT_{{{\text{p}},0}}^{2} /E_{\text{a}} }} $$
(5)
where γ = E a/(E a + 2RT max).
The datasheet of MCC-2 from Govmark® Organization Inc [2] correlates η c from MCC tests with the Limiting Oxygen Index (LOI, ASTM2863 test) and the Underwriters Laboratory (UL94) test for flammability of plastics. The relationship between η c and LOI can be described as [2]
$$ {\text{LOI}} = \frac{125}{{\left( {\eta_{\text{c}} } \right)^{1/4} }} $$
(6)
or from [4]
$$ {\text{LOI}} = 12 + \frac{4000}{{\eta_{\text{c}} }} $$
(7)
The corresponding ranges of η c and LOI are as follows [4]
  • η c ≥ 400 J g−1 K−1; no NR in the UL 94 vertical burn test and LOI < 25.

  • η c = 200–400 J g−1 K−1; self-extinguishing in UL test (V2/V1) and LOI = 25–30.

  • η c = 100–200 J g−1 K−1; self-extinguishing in UL test (V0/5 V) and LOI = 30–40.

  • η c ≤ 100 J g−1 K−1; no ignition (no after-flame in UL test) and LOI > 40.

η c is regarded as constant in many literatures or with small changes with deferent heating rate [3, 4, 13]. For example, in the literature [13], five polymers were tested over a wide range of heating rates, and the effect of heating rate on η c is about ± 10% over the range of heating rates, and is only about ± 4% over the range of heating rates β = 0.5–2 K s−1 typically used in MCC. But in our previous research [14], η c calculated according to ASTM D7309-13 was quite dependent on heating rate (1136.4 J g−1 K−1 at 10 K min−1, while 873.0 J g−1 K−1 at 100 K min−1) and also had large gap in the range of low heating rates. Different LOI and UL94 results would be calculated from Eqs. 6 and 7, and may lead to different classification of flammability of the same material. Thus, a series of MCC tests were arranged to investigate η c at different heating rates and screen suitable algorithms to derive η c.

Experiment

Facilities and material

MCC tests were conducted with a Govmark MCC-2 located at the VTT Research Center of Finland. Specifications of the Govmark MCC-2 instrument are as follows [2],
  1. 1.

    Sample heating rate: 0–10 K s−1

     
  2. 2.

    Gas flow rate: 50–200 cm3 min−1, response time of < 0.1 s, sensitivity of 0.1% of full scale,

     
  3. 3.

    Repeatability is ± 0.2% of full scale and an accuracy of ± 1% of full scale deflection.

     
  4. 4.

    Sample size: 0.5–50 mg (milligrams).

     
  5. 5.

    Detection limit: 5 mW.

     
  6. 6.

    Repeatability: ± 2% (10 mg specimen).

     

Pyrolyzer heating temperature was from 75 to 600 °C, and combustor temperature was set at 900 °C.

All tests followed “Method A” procedure of the MCC. In “Method A” procedure the specimen undergoes a controlled thermal decomposition [3] when subjected to controlled heating in an oxygen-free/anaerobic environment. The gases released by the specimen during operation are swept from the specimen chamber by nitrogen, subsequently mixed with excess oxygen, and then completely oxidized in a high temperature combustion furnace. The volumetric flow rate and volumetric oxygen concentration of the gas stream exiting the combustion furnace are continuously measured during the test to calculate the rate of heat release by means of oxygen consumption. In Method A, the heat of combustion of the volatile component of the specimen (specimen gases) is measured but not the heat of combustion of any solid residue [3].

From “Method A” procedure, the maximum HRR per unit mass q max, onset temperature T onset, temperature at maximum HRR per unit mass T max, total heat release h c, heat release capacity η c, and oxygen concentration at maximum heat release rate \( \Delta_{{{\text{O}}_{2} }} \) may be determined.

Preparation of specimen and choice of heating rate

The MCC tests were carried out for black PMMA and two kinds of extruded polystyrene (XPS). In the tests, 9 heating rates, 0.1, 0.2, 0.5, 1.0, 1.5, 2.0, 2.5, 3.0, and 3.5 K s−1, were selected. The PMMA is black and with density of 1180 kg m−3, a reference material for the cone calorimeter and the MCC at VTT. The prepared specimens were in three groups with nominal specimen masses of 1.00, 1.50, and 2.50 mg, and the standard error of each group is 0.034, 0.113, and 0.064 mg. LOI is from 17 to 19 [15, 16].

Two kinds of XPS foam panel were commonly used as exterior insulation finishing system in China. One is with gray color and a density of 37.8 kg m−3, which is labeled as XPS_grey. The oxygen index as measured by ASTM2863 is 20.5. Specimen was taken from the foam panel. The specimens were prepared in three groups with nominal specimen masses of 1.50, 2.50, and 3.50 mg, and the standard error of each group is 0.188, 0.101, and 0.159 mg.

The other one is with red color and a density of 52.6 kg m−3, which is labeled as XPS_red. The oxygen index as measured by ASTM2863 is 19.3. The specimens were also prepared in three groups with nominal specimen masses of 1.00, 1.50, and 2.00 mg, and the standard error of each group is 0.043, 0.052, and 0.055 mg.

Specimen mass was weighed by a Mettler AX205 AX-205 Analytical Semi Microbalance Delta Range with readability of 0.01 mg in the weighing range of 81 g. Totally 81 specimens were tested for these three materials.

Test results and analysis

Figures 13 illustrate the heat release rate of PMMA, XPS_grey, and XPS_red with nominal mass of 1.00, 2.00, and 3.50 mg.
Fig. 1

PMMA MCC tests (1.00 mg)

Fig. 2

XPS_grey_MCC tests (2.0 mg)

Fig. 3

XPS_red_MCC tests (3.50 mg)

As E a will be used in above equations, Kissinger plots [17] were used to calculate E a for these three materials, as shown in Figs. 46, and calculated results are listed in Table 1.
Fig. 4

PMMA energy

Fig. 5

XPS_grey energy

Fig. 6

XPS_red energy

Table 1

Calculated E a (k J mol−1) for each material

Specimen types

E a

average

σ

PMMA

 1.00 mg

159.1

162.4

8.7

 1.50 mg

172.3

 2.50 mg

155.8

XPS_grey

 1.50 mg

208.3

203.7

8.9

 2.50 mg

209.3

 3.50 mg

193.4

XPS_red

 1.00 mg

226.7

229.4

2.4

 1.50 mg

231.3

 2.00 mg

230.1

η c is calculated with Eqs. 1 and 4 (with β 0 = 1 K s−1) and shown in Figs. 79. η c depends on heating rate remarkably. The results from Eq. 1 have exponential relationship with β, which can be exponentially fitted by Eq. 8, and the fitting parameters are shown in Table 2.
$$ \eta_{\text{c}} = {\text{A}}1 \times {\text{e}}^{{\left( { - \beta /{\text{t}}1} \right)}} + \eta_{0} $$
(8)
Fig. 7

η c of PMMA from Eqs. 1 and 4

Fig. 8

η c of XPS_grey from Eqs. 1 and 4

Fig. 9

η c of XPS_red from Eqs. 1 and 4

Table 2

Parameters of exponential fitting of η 0 versus heating rates

Specimen types

A1

t1

η 0

R 2

PMMA

 1.00 mg

586.8

0.57

347.1

0.982

 1.50 mg

526.5

0.62

335.9

0.969

 2.50 mg

851.7

0.33

355.0

0.950

XPS_grey

 1.50 mg

520.2

1.29

309.7

0.994

 2.50 mg

500.0

0.98

329.3

0.982

 3.50 mg

490.7

1.25

307.2

0.982

XPS_red

 1.00 mg

1023.8

0.86

619.7

0.993

 1.50 mg

1135.1

0.81

636.0

0.983

 2.00 mg

1102.7

0.84

603.1

0.995

The results from Eq. 4 have the same tendency as those from Eq. 1 and also depend on β. The differences between the maximum and minimum η c calculated by both Eqs. 1 and 4 are very large; the ratios of maximum to minimum are around 2, as listed in Table 3. The curves of η c are quite different from those in the literature [13] and can’t be fitted linearly.
Table 3

Some of the calculated η c by Eqs. 15, and LOI by Eqs. 6 and 7

PMMA

1.00 mg

1.50 mg

2.50 mg

LOIa

LOIb

Equation 1

 Max

826.4

815.9

1036.2

22.9

16.5

 Min

341.5

304.0

337.1

29.4

24.2

 Mean

479.8

498.6

503.9

26.5

20.1

 Max/min

2.42

2.68

3.07

Equation 2

 Max

435.9

441.5

454.0

27.2

21.0

 Min

334.1

361.4

348.1

28.9

23.5

 Mean

369.1

393.4

362.3

28.4

22.7

 Max/min

1.30

1.22

1.30

Equation 3

 Max

386.7

411.1

399.3

28.0

22.0

 Min

351.8

372.5

341.1

28.8

23.3

 Mean

369.0

393.9

362.1

28.4

22.7

 Max/min

1.10

1.10

1.17

Equation 4

 Max

707.8

632.8

739.3

24.4

17.8

 Min

372.8

329.8

368.9

28.8

23.2

 Mean

483.7

457.6

472.0

26.8

20.5

 Max/min

1.90

1.92

2.00

Equation 5

 Max

410.7

436.8

424.8

27.6

21.4

 Min

373.1

394.3

363.3

28.4

22.6

 Mean

393.4

418.1

386.8

28.0

22.0

 Max/min

1.10

1.11

1.17

XPS_grey

1.50 mg

2.50 mg

3.50 mg

  

Equation 1

 Max

792.0

770.0

742.3

23.7

17.2

 Min

344.7

326.6

332.8

29.2

24.0

 Mean

512.3

505.6

508.3

26.3

19.9

 Max/min

2.30

2.36

2.23

Equation 2

 Max

456.2

471.2

432.5

27.1

20.8

 Min

382.3

379.9

383.7

28.3

22.5

 Mean

413.0

418.6

402.4

27.8

21.7

 Max/min

1.19

1.24

1.13

Equation 3

 Max

503.8

514.8

479.6

26.4

20.0

 Min

433.7

462.5

421.5

27.3

21.1

 Mean

478.9

493.6

464.4

26.7

20.4

 Max/min

1.16

1.11

1.14

Equation 4

 Max

695.6

676.6

645.2

24.6

18.0

 Min

370.9

351.3

360.2

28.7

23.1

 Mean

516.1

496.3

499.0

26.4

19.9

 Max/min

1.88

1.93

1.79

Equation 5

 Max

532.8

544.2

509.3

26.1

19.6

 Min

458.8

486.6

445.2

26.9

20.6

 Mean

505.5

520.9

492.3

26.4

19.9

 Max/min

1.17

1.12

1.14

XPS_red

1.00 mg

1.50 mg

2.00 mg

  

Equation 1

 Max

1528.1

1630.6

1585.0

19.8

14.5

 Min

615.1

626.3

580.4

25.2

18.6

 Mean

952.1

989.5

955.7

22.4

16.1

 Max/min

2.48

2.60

2.73

Equation 2

 Max

661.4

731.8

706.2

24.3

17.7

 Min

547.7

568.3

573.7

25.7

19.1

 Mean

598.7

629.7

616.7

25.1

18.5

 Max/min

1.12

1.18

1.17

Equation 3

 Max

688.2

702.9

659.2

24.5

17.9

 Min

568.9

631.6

622.9

25.2

18.6

 Mean

629.4

666.0

643.8

24.8

18.2

 Max/min

1.21

1.11

1.06

Equation 4

 Max

1357.4

1451.7

1410.1

20.4

14.8

 Min

657.6

668.5

619.9

24.8

18.2

 Mean

934.4

977.8

936.6

22.5

16.2

 Max/min

2.06

2.17

2.28

Equation 5

 Max

723.7

733.8

692.8

24.2

17.6

 Min

596.7

658.6

653.1

24.9

18.3

 Mean

661.4

695.6

676.1

24.5

17.9

 Max/min

1.21

1.11

1.06

aLOI calculated from Eq. 6

bLOI calculated from Eq. 7

For PMMA and grey XPS, some of the calculated η c lower than 400 and the others are higher than 400, and this would classify the same materials as both No NR in the UL 94 vertical burn test and LOI < 25, and also self-extinguishing in UL test (V2/V1) and LOI = 25–30.

Some literatures consider the peak heat release rate temperature as combustion temperature [3], or it is related to ignition temperature of a polymer [18] or the pyrolysis temperature [19] as at this point the pyrolysis temperature is reached. Peak heat release rate temperature in MCC tests is used as T p in Eq. 2.

Figure 10 illustrates all η c calculated from Eq. 2. Although η c decreases as heating rate increases generally, the dependence is very weak. The maximum, minimum η c, and their ratios are listed in Table 3.
Fig. 10

η c calculated from Eq. 2

Residue mass is considered in Eq. 2; thus, the measurement error of residue mass would influence the accuracy of calculated η c.

Figures 1116 illustrate η c calculated from Eqs. 3 and 5. Error bar shows the difference of η c at the same heat rate with a reference heating rate from 0.1 to 3.5 K s−1.
Fig. 11

η c of PMMA from Eq. 3

Fig. 12

η c of PMMA from Eq. 5

Fig. 13

η c of XPS_grey from Eq. 3

Fig. 14

η c of XPS_grey from Eq. 5

Fig. 15

η c of XPS_red from Eq. 3

Fig. 16

η c of XPS_red from Eq. 5

Maximum, minimum, and mean of η c calculated by all equations are listed in Table 3, and the ratios of maximum to minimum η c are also listed. The ratios are less than 1.20 from Eqs. 2, 3, and 5. η c of PMMA is from 350 to 450 J g−1 K−1, also corresponding to two classifications of flammability.

The averages of η c calculated by Eqs. 2, 3, and 5 are listed in Table 4. The LOI calculated from Eq. 7 is closer to test results.
Table 4

Average η c from Eqs. 2, 3, and 5

Material

Equation 2

Equation 3

Equation 5

HRC/J g−1 K−1

σ/J g−1 K−1

HRC/J g−1 K−1

σ/J g−1 K−1

HRC/J g−1 K−1

σ/J g−1 K−1

PMMA

374.9

16.4

375.0

16.7

399.4

16.5

LOIa

28.4

28.4

28.0

LOIb

22.7

22.7

22.0

XPS_grey

411.3

8.25

479.0

14.6

506.3

14.3

LOIa

27.8

26.7

26.4

LOIb

21.7

20.4

19.9

XPS_red

615.1

15.6

646.4

18.4

677.7

17.2

LOIa

25.1

24.8

24.5

LOIb

18.5

18.2

17.9

aLOI calculated from Eq. 6

bLOI calculated from Eq. 7

Conclusions

From the above analysis, Eqs. 1 and 4 are not suitable for the calculation of the η c, and both algorithms are dependent on heating rate strongly. Even the so-called rate-independent algorithms will get different calculated results because of heating rates or reference heating rates. Equations 2, 3, and 5 can be used to calculate η c. But heating rate β and reference heating rate β 0 must be mentioned when present the η c derived from MCC tests. Specimen mass also influences the result from MCC. Specimen mass in the same experiment group should be as close as possible. η c is correlated with LOI and can be used to estimate LOI. The accurate relationship between η c and LOI requires further study. Algorithm, heating rate, specimen mass, and test errors can affect the accuracy of η c.

Notes

Acknowledgements

This research is supported by the Natural Science Fund of China, Nos. 51376093 and 51776098. The research team is honored by “Six Talent Peaks” project of Jiangsu Province, China.

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Copyright information

© Akadémiai Kiadó, Budapest, Hungary 2017

Authors and Affiliations

  • Qiang Xu
    • 1
  • Cong Jin
    • 2
  • Andrea Majlingova
    • 3
  • Agoston Restas
    • 4
  1. 1.School of Mechanical EngineeringNanjing University of Science and TechnologyNanjingChina
  2. 2.School of Computer Science and TechnologyNanjing University of Science and TechnologyNanjingChina
  3. 3.Faculty of Wood Science and TechnologyTechnical University in ZvolenZvolenSlovakia
  4. 4.Department of Fire Prevention and Rescue ControlNational University of Public ServiceBudapestHungary

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