LAPORAN TEKNIS INTERN

PUSAT TEKNOLOGI PENERBANGAN

LITERATURE STUDY REVIEW: CURED PLY THICKNESS (CPT) METHOD FOR FIBER
REINFORCE POLYMER COMPOSITE

RIAN SUARI ARITONANG, ST

NO :
LITERATURE STUDY REVIEW: CURED PLY THICKNESS (CPT)
METHOD FOR FIBER REINFORCE POLYMER COMPOSITE

Oleh :
Rian Suari Aritonang, ST

PUSAT TEKNOLOGI PENERBANGAN

DEPUTI BIDANG TEKNOLOGI PENERBANGAN DAN ANTARIKSA
LEMBAGA PENERBANGAN DAN ANTARIKSA NASIONAL
2020
 LEMBAGA PENERBANGAN DAN ANTARIKSA NASIONAL
(LAPAN)

JI. Raya LAPAN, Rumpin Bogor, Jawa Barat

Telp. (021) 757 00383, 757 90031, Fax. (O21)75790383

SURAT — TUGAS
NOMOR : /02/2020

a. bahwa dalam rangka melaksanakan .

b. bahwa pegawai yang namanya tercantum dalam Surat Tugas ini di
Menimbang tunjuk untuk melaksanakan kegiatan sebagaimana di maksud dalam
huruf a:

1. Peraturan Kepala Lembaga Penerbangan dan Antariksa Nasional

Nomor 8 Tahun 2015 tentang Organisasi dan Tata Kerja Kepala
Lembaga Penerbangan dan Antariksa Nasional (Berita Negara
Dasar Republik Indonesia Tahun 2017 Nomor 1573) sebagaimana telah
diubah dengan peraturan Lembaga Penerbangan dan Antariksa
Nasional Nomor 08 Tahun 2017 (Berita Negara Republik Indonesia
Tahun 2017 Nomor 1573);
2. Keputusan Kepala Lapan Nomor tentang Pengangkatan
Pegawai Negeri Sipil dalam Jabatan Struktural:

Memberikan Tugas

Kepada 1.
NIP
Penata Muda Tk. I — III/a

Untuk 1. Melaksanakan kegiatan tersebut di Pustekbang LAPAN.

2. Melaksanakan tugas dengan sebaik - baiknya dan penuh rasa
tanggung jawab:
3. Memberikan laporan atas hasil pelaksanaan tugas tersebut kepada
atasan masing - masing

Dikeluarkan di Rumpin
Pada tanggal, 29 Februari 2020

Mengetahui,
Kepala Pusat Teknologi Penerbangan

Drs. Gunawan Setyo Prabowo, M.T.

NIP. 19670724 199203 1 002
1. Nomor / Tahun Terbit: 2. Jenis Terbitan: 3. Nomor Penugasan
Laporan Teknis Intern
5. Tanggal Pelaporan
4. Judul :

Literature Study Review: Cured Ply Thickness (Cpt) Method For Fiber
Reinforce Polymer Composite

6. Penulis: 7. Editor:

Rian Suari Aritonang, ST

198811292018011002
8. Organisasi Pelaksana (OP) 9. Periode Pelaksanaan:
Bidang Aerostruktur, Pusat Teknologi Penerbangan
10. Abstrak :

Dokumen ini merupakan dokumen study review Metode Cured Ply Thickness (CPT) untuk
material komposit matriks polimer berpenguat serat. Tujuan dokumen ini untuk
mengetahui metode CPT dan constituent content yang digunakan pada bahan komposit.
Dengan mengetahui komposisi dari unsur unsur penyusun komposit yaitu serat dan
matriks maka dapat membantu dalam analisis sifat mekanik, sifat fisik, sifat termal
maupun sifat elektrikalnya yang nilai dipengaruhi oleh serat dan matriks pada komposit.
Volume void yang diperoleh dari metode penentuan ini bertujuan untuk melihat nilai
besaran volume void yang dihasilkan dan efeknya pada sifat mekanik komposit. Semakin
besar nilai volume void maka semakin rendah nilai sifat mekaniknya dan rentan terhadap
adanya proses penyerapan kelembaban dan pengaruh lingkungan basah sehingga nilai
sifat mekanik komposit yang dihasilkan bervariasi tinggi.

11. Kata-Kata Penting: 12. Persetujuan Pejabat Berwenang

CPT Kepala Bidang Program dan Fasilitas

Density
Fiber Content
Matriks/ Matrix Content
Ir. Agus Aribowo, M.Eng
197008071989011001

13. Klasifikasi: 14. Distribusi: 15. Kategori Subyek: 16. Jumlah Halaman:
Biasa iTak Terbatas
LITERATURE STUDY REVIEW: CURED PLY THICKNESS (CPT) METHOD FOR
FIBER REINFORCE POLYMER COMPOSITE

1. Pendahuluan
Dokumen ini merupakan dokumen study review Metode Cured Ply Thickness (CPT) untuk
material komposit matriks polimer berpenguat serat. Tujuan dokumen ini untuk
mengetahui metode CPT dan constituent content yang digunakan pada bahan komposit.
Dengan mengetahui komposisi dari unsur unsur penyusun komposit yaitu serat dan
matriks maka dapat membantu dalam analisis sifat mekanik, sifat fisik, sifat termal
maupun sifat elektrikalnya yang nilai dipengaruhi oleh serat dan matriks pada komposit.
Volume void yang diperoleh dari metode penentuan ini bertujuan untuk melihat nilai
besaran volume void yang dihasilkan dan efeknya pada sifat mekanik komposit. Semakin
besar nilai volume void maka semakin rendah nilai sifat mekaniknya dan rentan terhadap
adanya proses penyerapan kelembaban dan pengaruh lingkungan basah sehingga nilai
sifat mekanik komposit yang dihasilkan bervariasi tinggi.

2. Tujuan Kegiatan
Dokumen ini menjelaskan mengenai study review Metode Cured Ply Thickness (CPT)
untuk material komposit yang bertujuan untuk mengetahui metode Cured Ply Thickness
(CPT) yang digunakan pada material komposit dan penentuan constituent content pada
komposit berpenguat serat matriks polimer berpenguat serat.

Singkatan dan Defenisi

Constituent material makro dasar penyusun komposit; fiber, matriks
CPT Cured Ply Thickness
Fiber Content Jumlah serat yang ada pada komposit (%w, atau %V)
Matrix Cotent Jumlah matriks yang ada pada komposit (%w atau %V)
Void Volume Volume pada spesimen tanpa kandungan massa serat/matriks
Density satuan berat per unit volume di udara pada suhu 23 deg C.

3. Kegiatan: Study Review

Terdapat beberapa beberapa metode dalam menentukan kandungan unsur penyusun
pada suatu material komposit matriks polimer berpenguat serat atau Fiber Reinforce
Polymer / FRP Composite. Pada ASTM D3171 menyebutkan terdapat dua metode dalam
menentukan unsur penyusun tersebut (baca: Matriks, Serat penguat, dan void). Metode
I secara sederhana adalah menghilangkan unsur matriks pada komposit melalui cara
pelarutan atau proses pembakaran atau proses karbonisasi dengan menyisakan unsur
penyusun serat penguat dengan catatan proses itu tidak mempengaruhi perhitungan
jumlah kandungan baik perhtiungan jumlah kandungan berat dan volumenya.
Metode II hanya dapat digunakan pada jenis laminat FRP Composite yang sudah di
ketahui nilai dari area weigth (berat per satuan luas) dari serat. Kelemahannya, Metode
II tidak dapat di gunakan pada perhitungan volume void yang dihasilkan pada proses
manufaktur.
4. Hasil Kegiatan
4.1 Test Method I
Prosedur metode test I adalah menghilangkan massa dari matriks denga media larutan
pelarut, atau tungku bakar. Ketika pelarutan berlangsung dengan menggunakan media
larutan (hot liquid medium) menghasilkan sisa residu yang menyisakan kandungan serat
pada komposit yang kemudian di saring, di bersihkan, dikeringkan dan didinginkan lalu
di hitung jumlah beratnya. Dengan adanya data densitas baik dari densitas serat dan
densitas komposit dan data dari jumlah persen massa yang terhitung dari serat sisa tadi
maka bisa didapat nilai persen volume. Perhitungan tambahan pada volume void dapat
dilakukan dengan terlebih dahulu didapat nilai dari densitas matriks.
Prosedur yang dilakukan pada test metode I terbagi pada 8 prosedur yaitu:
1) Prosedur A, untuk matriks seperti epoxy, phenolic, polyamide dan jenis resin
yang dapat larut pada asam nitrat. Penggunaan reflux condenser untuk
mengkondesasi ulang materi matriks yang mengalami penguapan.

2) Prosedur B, dapat digunakan pada matriks seperti epoxy, phenolic, polyamide

dan jenis resin termoplastik lain yang dapat larut pada larutan campuran asam
sulfur dan hydrogen peroksida.

3) Prosedur C, untuk matriks seperti epoxy resin dan resin lain yang dapat larut
pada campuran ethylene glycol dan potassium hidroksida. Penggunaan reflux
condenser untuk mengkondesasi ulang materi matriks yang mengalami
penguapan

4) Prosedur D, untuk matriks aluminum, paduan tembaga, dan matriks yang dapat
dilarutkan pada larutan sodum hidroksida.

5) Prosedur E, digunakan pada matriks baja, titanium, tembaga, aluminum, dan lain
yang bisa dilarutkan oleh asam Hidroklorik.

6) Prosedur F, prosedur ini adalah pengembangan prosedur A dengan tambahan

prosedur pemanasan dengan microwave.

7) Prosedur G, cocok untuk komposit berpenguat serat gelas, atau serat keramik
lainnya yang tidak terpengaruh pada lingkungan temperature tinggi.Kondisi
temperature tinggi diperoleh dari muffle furnace pada suhu 600 ± 30 deg.
Celcius.

8) Prosedur H, cocok untuk jenis penguat apa saja, biasanya digunakan pada serat
karbon, yang mana serat tersebut tidak terpengaruh pada kondisi temperature
tinggi pada lingkungan nitrogen. Kondisi suhu tinggi ber lingkungan nitrogen
diperoleh pada penggunaan Nitrogen-Purging Furnace pada temperatur
operasional 560 ± 40 deg. Celsius. Pada suhu tersebut matriks dari komposit
serat karbon terkarbonisasi karena lingkungan nitrogen tungku.
Peralatan lab yang umum digunakan:
1) Thermal Shock (Tempered Glass atau PTFE material)

2) Post Test Elemental Analysis

3) Tungku (Muffle Furnace)

Gambar 1 Muffle Furnace

4) Timbangan (Analytical Balance) dengan ketelitian ±0,1 mg

Gambar 2 Analytical Balance

5) Desiccator Lab.
 Gambar 3 Desiccator Lab.
6) Perlengkapan Alat Pemanas (Heating Mantle, Hot Plate, atau temperature
bath yang dapat di atur suhu dengan konsistensi fluktuasi temperatur ± 10
deg. Celsius)

Gambar 4 Alat Pemanas Lab

7) Drying Oven yang dapat menjaga suhu pada 100± 3 deg. Celsius atau
temperatur yang diinginkan pada rentang fluktuasi ±3 deg C.

8) Sampel Container, Gelas Beaker, Gelas Borosilicate min. 50 mL.

9) Vaccum Pressure pada min. 50 kPa

10) Alat filtrasi (Filtering Apparatus)

Gambar 5 Filtering Apparatus

 11) Reflux Condenser untuk mengkondensasi materi matriks yang menguap

Gambar 6 Reflux Condenser

12) Alat lab pelengkap seperti: Pipet, beaker, Watchglass, dan lint free Wipes

Gambar 7 Alat Lab Pelengkap

4.2 Test Spesimen Test Method I

Jumlah spesimen yang dianjurkan adalah minimum berjumlah 3 spesimen. Spesimen
yang digunakan adalah spesimen yang pemotongan dan ukuran yang sama. Spesimen
paling tidak memiliki jumlah massa yang tidak kurang dari 0,5 gram dan minimal 1,0
gram jika perhitungan void dilakukan. Tidak ada ketentuan khusus dalam hal bentuk
spesimen. Spesimen yang sama digunakan pada penentuan densitas dan penetuan
volume serat.
Spesimen harus terbebas dari minyak, gemuk, dan benda asing lainnya. Pada proses
pemotongan sebaiknya dihindarkan tipe pemotongan yang dapat menyebabkan
delaminasi pada spesimen komposit. Pemotongan yang tidak benar akan menyebabkan
adanya udara terjebak pada spesimen dan menyebabkan salah pada perhitungan
densitas.
Pengkondisian pada spesimen dilakukan setelah spesimen selesai dari tahap
pemotongan. Pengkondisian spesimen uji adalah dengan melakukan pengeringan
 spesimen pada kondisi equilibrium nya sesuai dengan prosedur pada metode uji ASTM
D5229/ D5229M.
Kondisi pengujian dilakukan pada temperatur 23 ± 5 deg. C. dan kondisi kelembaban
udara pada maksimal pada 65 % RH. Spesimen uji untuk pengujian densitas dikondisikan
pada 10 menit setelah di ambil dari dessicator.

4.3 Calculation Test Method I

Tahapan perhitungan (Calculation) pada metode test I dilakukan untuk perhitungan
pada (untuk Prosedur A sampai dengan Prosedur G):
1. Kandungan Serat Penguat (Persen Berat %W)

2. Kandungan Serat Penguat (Persen Volume %V)

3. Kandungan Resin Matriks Pengikat (Persen Berat %W)

4. Kandungan Resin Matriks Pengikat (Persen Volume %V)

5. Volume Void (Persen Volume %V)

Untuk Prosedur H pada metode test I,yaitu:

1. Rasio Karbonisasi pada resin

2. Massa resin matriks pada spesimen komposit

3. Kandungan Serat Penguat (Persen Berat %W)

4. Kandungan Serat Penguat (Persen Volume %V)

5. Kandungan Resin Matriks Pengikat (Persen Berat %W)

6. Kandungan Resin Matriks Pengikat (Persen Volume %V)

7. Volume Void Spesimen (Persen Volume %V)

4.4 Test Method II

Berbeda dari metode test I, metode test II tidak dapat melakukan atau tidak applicable
untuk perhitungan volume void pada spesimen komposit. Pada metode test II,
dibutuhkan data nilai berat per satuan luas atau area dari serat penguat. Diasumsikan
dan dianggap void tidak diperhitungkan.
Metode test II secara umum prosedur pengujiannya adalah dengan melakukan
pengukuran ketebalan relatif dari panel komposit berserat penguat dan nilai berat per
satuan luas (Areal Weight) dari serat penguat. Dari pengukuran tebal panel komposit,
kandungan serat penguat dan kandungan resin matriks pengikat dapat dihitung.
 Peralatan yang digunakan pada metode test II adalah:
1. Alat ukur ketebalan (Thickness Measuring Device). Dapat berupa micrometer atau
indicator digital dengan kemampuan resolusi pembacaan pada 0,001 mm.

Gambar 8 Micrometer Digital

2. Caliper, dapat mengukur pembacaan ukuran panjang atau lebar pada 0,1%
akurasi. Kemampuan Pembacaan Panjang dari caliper bervariasi mulai dari 75 mm
sampai dengan 1500 mm.

Gambar 9 Caliper

4.5 Test Spesimen Test Method II

Jumlah spesimen yang dianjurkan adalah minimum berjumlah 1 spesimen. Geometri dari
spesimen uji adalah dimensi dari panel komposit. Minimum spesimen area permukaannya
adalah pada 625 mm2 (25 mm x 25 mm) untuk geometri cuboid. Spesimen harus terbebas
dari minyak, gemuk, atau benda asing lainnya. Setelah tahapan pemotongan, sampel di
kondisikan sesuai dengan prosedur pada metode uji ASTM D5229/ D5229M.
Adapun prosedur dari pengujian metode test II adalah:
1) Perhitungan massa spesimen

2) Penentuan densitas mengacu pada ASTM D0792

3) Penghitungan ketebalan spesimen paling tidak satu kali pada permukaan

yang tidak beraturan. Perhitungan dilakukan sebanyak 10 kali dengan nilai
rata rata diambil sebagai nilai representatif.

4) Penggunaan caliper untuk menghitung ukuran Panjang dan lebar spesimen.

Penghitungan ukuran Panjang dan lebar dilakukan sebanyak tiga kali. Nilai
representatif dari Panjang dan lebar adalah diambil dari nilai rata rata.
 4.6 Calculation Test Method II
Tahapan perhitungan (Calculation) pada metode test II dilakukan untuk perhitungan
pada:
1) Densitas Spesimen (gr/cm3)

2) Kandungan Serat Penguat (Persen Berat %W)

3) Kandungan Serat Penguat (Persen Volume %V)

4) Kandungan Resin Matriks Pengikat (Persen Berat %W)

5) Kandungan Resin Matriks Pengikat (Persen Volume %V)

6) Cured Ply Thickness (CPT), mm

5. Referensi

1. ASTM D3171-15 The Standard Test Method for Constituent Content of Composite
Materials
2. ASTM D0792 Test Method for Density and Specific Gravity (Relative Density) of Plastic
3. ASTM D3878 Terminology for Composite Materials
6. Appendiks
 D3171 − 15
13.1.2.2 Perform the full test procedure on blank.
13.1.2.3 The mass difference between the original blank
mass and the mass after digestion or combustion divided by the
original blank mass is the reinforcement fractional loss or gain.
13.1.2.4 This fractional loss (or gain), if reproducible, may
be added (or subtracted) to the equation in 14.1.1 or 14.2.3.
13.1.2.5 Only fractional differences larger than 0.005
(0.5 %) shall be considered significant.
13.1.3 Correction for Matrix Weight Change:
13.1.3.1 Weigh one blank consisting only of cured matrix.
The blank mass shall roughly equal the mass of matrix in the
test specimens to the nearest 0.0001 g.
13.1.3.2 Perform the full test procedure on blank.
13.1.3.3 Since all matrix should be removed, the mass after
digestion or combustion divided by the original blank mass is
the matrix residue. This represents matrix material not re-
moved by digestion or combustion.
13.1.3.4 This fractional gain, if reproducible, may be added
to the equation in 14.1.3.
13.1.3.5 Only fractional differences larger than 0.005
(0.5 %) shall be considered significant.
13.2 Test Method II:
13.2.1 Weigh each specimen to the nearest 0.0001 g.
13.2.2 Determine the density of each specimen in accor-
dance with Test Methods D792 or D1505 or use the calculation
shown in 14.3, if fiber volume percent or void percent, or both,
are required. The preconditioning for D792 or D1505 speci-
mens is to be in accordance with D3171 Section 12.
13.2.3 A micrometer with a 4 to 7 mm [0.16 to 0.28 in.]
nominal diameter ball interface shall be used to measure the
specimen thickness when at least one surface is irregular (such
as the bag-side of a laminate). A micrometer with a 4 to 7 mm
[0.16 to 0.28 in.] nominal diameter ball interface or with a flat
anvil interface shall be used to measure the specimen thickness
when both surfaces are smooth (such as tooled surfaces).
Measure thickness in at least ten locations. Take the average
measurement to determine the specimen thickness.
13.2.4 A micrometer or caliper, with a flat anvil interface,
shall be used to measure the length and the width of the
specimen. The accuracy of the instruments shall be suitable for
reading to within 1 % of the sample dimensions. For typical
specimen geometries, an instrument with an accuracy of
60.0025 mm [60.0001 in.] is adequate for the thickness
measurement, while an instrument with an accuracy of
60.025 mm [60.001 in.] is adequate for the length and the
width measurement. Measure the specimen width and length in
at least three locations. Take the average of the measurements
to determine the length and width.
14. Calculation
14.1 Test Method I, Procedures A through G:
14.1.1 Reinforcement Content, Weight Percent—Calculate
reinforcement content, in weight percent in accordance with Eq
1.
W r 5 ~ M f /M i ! 3 100 (1)
where:
Mi = initial mass of the specimen, g and
6
Mf = final mass of the specimen after digestion or
combustion, g.
NOTE 4—The mass of the fiber may be obtained by taking the mass of
the crucible with reinforcement minus the crucible mass (Mf = Mcr – Mc).
14.1.2 Reinforcement Content, Volume Percent—Calculate
reinforcement content, in volume percent, in accordance with
Eq 2.
V r 5 ~ M f /M i ! 3 100 3 ρ c /ρ r (2)
where:
ρr = density of the reinforcement, g/cm3 and
ρc = density of the specimen, g/cm3.
14.1.3 Matrix Content, Weight Percent—Calculate matrix
content, in weight percent, in accordance with Eq 3.
W m 5 ~ M i 2 M f ! /M i 3 100 (3)
14.1.4 Matrix Content, Volume Percent—Calculate matrix
content, in volume percent, in accordance with Eq 4.
V m 5 ~ M i 2 M f ! /M i 3 ρ c /ρ m 3 100 (4)
where:
ρm = density of the matrix, g/cm3.
14.1.5 Void Volume—Calculate void volume, in percent, in
accordance with Eq 5.
V v 5 100 2 ~ V r 1V m ! (5)
NOTE 5—Negative values of Vv shall be reported. Values of void volume
more negative than –0.2 % indicate a potential testing problem; input
values and test procedure shall be investigated. See 6.1.
14.2 Test Method I, Procedure H:
14.2.1 Carbonization Ratio of the Neat Resin—Calculate
the carbonization ratio of the neat resin, CR, in accordance with
Eq 6:
CR 5 m d ⁄m i (6)
where:
md = final mass of the neat resin residue after carbonization,
g, and
mi = initial mass of the neat resin specimen, g
NOTE 6—The mass of the neat resin residue after carbonization may be
obtained by taking the mass of the crucible with residue minus the crucible
mass (md = mcr– mc). If there is no residue from neat resin specimen after
carbonization, CR is equal to zero since md is equal to zero.
14.2.2 Mass of the Resin Matrix in the Composite
Specimen—Calculate the mass of the resin matrix in the
composite specimen, in grams, in accordance with Eq 7:
M m 5 ~ M i 2 M d ! ⁄ ~ 1 2 CR ! (7)
where:
Mi = initial mass of the composite specimen, g, and
Md = final residue mass of the composite specimen, g
NOTE 7—The mass of the composite specimen residue after carboniza-
tion may be obtained by taking the mass of the crucible with residue minus
the crucible mass (Md = Mcr–Mc). “M” represents any mass associated
with fiber reinforced composite specimens while “m” the mass related to
neat resin specimens.
14.2.3 Reinforcement Content, Weight Percent—Calculate
reinforcement content in the composite specimen, in weight
percent, in accordance with Eq 8:
 D3171 − 15
W r 5 ~ M i 2 M m ! ⁄M i 3 100 14.3.6 Cured Ply Thickness, mm—Calculate the cured ply
5 ~ M d 2 M i 3 CR ! ⁄ ~ M i 3 ~ 1 2 CR !! 3 100 (8) thickness from the measured laminate thickness, h, in section
13.2.3, in accordance with Eq 17.
14.2.4 Reinforcement Content, Volume Percent—Calculate
h p 5 h/N p (17)
reinforcement content, in volume percent, in accordance with
Eq 9. where:
V r 5 ~~ M i 2 M m ! ⁄ M i ! 3 100 3 ρ c ⁄ρ r (9) hp = cured ply thickness, mm, and
Np = number of plies in the laminate.
where:
14.4 Statistics—For each series of tests, calculate the aver-
ρr = density of the reinforcement, g/cm3 and
ρc = density of the composite specimen, g/cm3 age value, standard deviation, and coefficient of variation (in
percent) of all values obtained:
14.2.5 Matrix Content, Weight Percent—Calculate matrix
content, in weight percent, in accordance with Eq 10. x̄ 5 S D
n
Σ x i ⁄n
i51
(18)
W m 5 M m ⁄M i 3 100 (10)

14.2.6 Matrix Content, Volume Percent—Calculate matrix S n21 5 ŒS n

i51
D
Σ x i2 2 n x̄ 2 ⁄ ~ n 2 1 ! (19)
content, in volume percent, in accordance with Eq 11. CV 5 100 3 S n21 ⁄x̄ (20)
V m 5 ~ M m ⁄ M i ! 3 100 3 ρ c ⁄ρ m (11)
where:
where: x̄ = sample mean (average),
ρm = density of the matrix, g/cm3 Sn-1 = sample standard deviation,
n = number of specimens,
14.2.7 Void Volume—Calculate void volume, in percent, in xi = measured or derived property, and
accordance with Eq 5. CV = sample coefficient of variation, in percent
NOTE 8—Negative values of Vv shall be reported. Values of void
volume more negative than –0.2 % indicate a potential testing problem; 15. Report
input values and test procedure shall be investigated. See 6.1. 15.1 Report the following information, or references point-
14.3 Test Method II: ing to other documentation containing this information, to the
14.3.1 Specimen Density, g/cm3—Calculate specimen den- maximum extent applicable:
sity in grams per cubic centimeter with Eq 12 or use equivalent 15.1.1 Reporting of terms that are beyond the control of a
test methods such as Test Methods D792 or Test Method given testing laboratory, such as material details, shall be the
D1505. responsibility of the requestor.
15.1.2 Revision level or date of issue of this test method.
ρ c 5 M i / ~ A 3 h 3 1000! (12)
15.1.3 Actual test procedure used.
where: 15.1.4 Any variations to this test method, anomalies noticed
Mi = mass of the specimen, g; during testing, correction factors, or any equipment problems
A = area of the specimen, m2; and that occurred during testing.
h = thickness of the specimen, mm. 15.1.5 Complete identification of the material tested includ-
ing type, source, form, and dimensions (see Guide E1309).
14.3.2 Reinforcement Content, Weight Percent—Calculate
15.1.6 Fiber density values used, and their source.
the reinforcement content in weight percent in accordance with
15.1.7 Individual and average values and standard devia-
Eq 13.
tions of reinforcement and matrix weight and reinforcement
W r 5 ~ A r 3 N 3 0.1! / ~ ρ c 3 h ! (13) and matrix volume percent.
where: 15.1.8 Individual and average value and standard deviation
for void percent.
Ar = mass of one sheet of reinforcement/unit area, g/m2 and
Np = number of sheets/plies in the test specimen. 15.1.9 Matrix density value used and source of value.
15.1.10 Drying times and oven temperature for both origi-
14.3.3 Reinforcement Content, Volume Percent—Calculate nal specimen drying (before density determination and after
the reinforcement content in volume percent in accordance digestion).
with Eq 14. 15.1.11 Exposure time for Procedure A8.
V r 5 ~ A r 3 N 3 0.1! / ~ ρ r 3 h ! (14) 15.1.12 For Test Method II, measurement equipment used,
individual and average laminate thickness width and length
14.3.4 Matrix Content, Weight Percent—Calculate the ma- measures.
trix content in weight percent in accordance with Eq 15. 15.1.13 Cured ply thickness from Test Method II, including
W m 5 100 2 ~~ A r 3 N 3 0.1! / ~ ρ c 3 h !! (15) individual and average values.
14.3.5 Matrix Content, Volume Percent—Calculate the ma- 16. Precision and Bias
trix content in volume percent in accordance with Eq 16. 16.1 Precision—The data required for the development of a
V m 5 W m 3 ρ c /ρ m (16) precision statement is not available for this test method.

7
 D3171 − 15
Committee D-30 is currently planning a round-robin test series
for this test method in order to determine precision.
16.2 Bias—Bias cannot be determined for this test method
as no accepted reference standard exists.
ANNEXES
(Mandatory Information)
A1. PROCEDURE A—MATRIX DIGESTION USING NITRIC ACID
Warning—Understand the hazards described in Section 9
before working with acids.
A1.1 Weigh each specimen, Mi, to the nearest 0.0001 g.
A1.2 Determine the density of each specimen in accordance
with Test Methods D792 or Test Method D1505 if fiber volume
percent or void percent, or both, are required. The precondi-
tioning for D792 or D1505 specimens is to be in accordance
with D3171 Section 12.
NOTE A1.1—Specimens may require further dicing or grinding before
digestion. After machining, specimens should be reweighed. Care should
be taken that the diced or ground specimen represents original sample
composition.
A1.3 Place each specimen in a separate flask or beaker
containing at least 30 mL of 70 % nitric acid.
A1.4 Constant heating with heating mantle, hot plate, or
controlled temperature bath is recommended. Temperature
requirements depend on the system to be digested. Generally,
temperatures should not exceed 80°C. (Warning—Reflux
condensers are recommended if the temperature exceeds
40°C.)
A2. PROCEDURE B—MATRIX DIGESTION USING SULFURIC ACID/HYDROGEN PEROXIDE
Warning—Understand the hazards described in Section 9
before working with acids.
A2.1 Weigh each specimen (Mi) to the nearest 0.0001 g.
A2.2 Determine the density of each specimen in accordance
with Test Methods D792 or D1505 if fiber volume percent or
void percent, or both, are required. The preconditioning for
D792 or D1505 specimens is to be in accordance with D3171
Section 12.
A2.3 Place each specimen into a 100-mL [minimum] bea-
ker.
8
17. Keywords
17.1 composite materials ; fiber content; matrix content;
reinforcement content; resin content; void volume
A1.5 The maximum time for digestion should be 6 h.
Shorter times are dependent on the composite system. The
matrix is considered fully digested if no trace of the
reinforcement/matrix laminate combination remains.
Unfortunately, this is difficult to detect until the specimen has
been removed from the digestion media.
A1.6 Filter the contents into tared or preweighed (Mc)
sintered glass filters (or filter-lined crucibles) under a vacuum
of 17 kPa or better. Wash the fiber three times with distilled
water. An acetone wash may be used as the final wash after
nitric acid is removed from the specimen to improve drying
times.
A1.7 Place the specimen in an oven at 100°C minimum
until the sample is dried (approximately 1 h at 100°C).
A1.8 Cool the filter or crucible to room temperature in a
desiccator. Weigh the specimen in its holder, Mcr, to the nearest
0.0001 g.
A2.4 Add a minimum of 20-mL sulfuric acid.
(Warning—Do not use less than 20-mL acid.) Place the beaker
on a hot plate and heat until the mixture starts to fume.
A2.5 After the solution is dark (with no appreciable change
in color for 5 min) add 50 or 30 % hydrogen peroxide down the
side of the beaker to oxidize the matrix. (Warning—This
procedure increases acid fumes. Wear rubber gloves, labora-
tory coat, and eye protection.) Typically, about 35 mL or more
of hydrogen peroxide are added. The fibers float to the top of
the solution, and the solution appears clear or color intensity
dramatically fades.
 D3171 − 15
A2.6 Remove the beaker from the hot plate and allow the
solution to cool. Cooling may be facilitated by a water or ice
bath. Any nondigested laminate should be clearly visible at this
point. If the matrix is not digested, the solution may be filtered,
then reintroduced into the beaker. Steps A2.4 – A2.6 may be
repeated.
A2.7 Filter the contents into tared or preweighed, Mc,
sintered glass filters (or filter-lined crucibles) under a vacuum
of 17 kPa or better. Wash the fibers three times with distilled
A3. PROCEDURE C—MATRIX DIGESTION USING ETHYLENE GLYCOL/POTASSIUM HYDROXIDE
Warning—Understand the hazards described in Section 9
before working with caustics.
A3.1 Weigh each specimen, Mi, to the nearest 0.0001 g.
A3.2 Determine the density of each specimen in accordance
with Test Methods D792 or D1505 if fiber volume percent or
void percent, or both, are required. The preconditioning for
D792 or D1505 specimens is to be in accordance with D3171
Section 12.
A3.3 Preparation of Reagent—Prepare a 10 % solution of
potassium hydroxide in ethylene glycol. (For example: Place
100 g of solid potassium hydroxide into a 1500-mL volumetric
flask. Add 500 mL of ethylene glycol. Heat gently to dissolve
the solid. Then add another 500 mL of ethylene glycol for a
total volume of 1 L.) Label and store flask.
A3.4 Place each specimen into a separate 250-mL flask and
add 100 mL of the potassium hydroxide-ethylene glycol
solution to each flask. Alternate solution volumes may be used
as long as the ratio of the components remains equivalent.
A3.5 Connect the flask to a reflux condenser. Start the
cooling water flow and adjust the temperature of the hot plate
or heating mantle to bring the solution to a gentle boil.
A4. PROCEDURE D—MATRIX DIGESTION USING SODIUM HYDROXIDE
Warning—Understand the hazards described in Section 9
before working with caustics.
A4.1 Weigh each specimen, Mi, to the nearest 0.0001 g.
A4.2 Determine the density of each specimen in accordance
with Test Methods D792 or D1505 if fiber volume percent or
void percent, or both, are required. The preconditioning for
D792 or D1505 specimens is to be in accordance with D3171
Section 12.
9
water. An acetone wash may be used as the final wash after
sulfuric acid and hydrogen peroxide is removed from the
specimen to improve drying times.
A2.8 Place the specimen in an oven at 100°C minimum
until the sample is dried (approximately 1 h at 100°C).
A2.9 Cool the filter or crucible to room temperature in a
desiccator. Weigh the specimen in its holder, Mcr, to the nearest
0.0001 g.
A3.6 Boil until the matrix is completely digested. An
indicator is when fibers separate and appear to float freely in
the solution.
A3.7 Remove the beaker from the reflux condenser.
NOTE A3.1—Because potassium hydroxide will attack the glass filter, it
is advisable to precondition the filter by pouring a small amount of
potassium hydroxide-ethylene glycol solution onto the filter.
A3.8 Filter the contents into tared or preweighed (Mc)
sintered glass filters under a vacuum of 17 kPa or better. Wash
the fiber two times with dimethylformamide, and three addi-
tional times with distilled water. An acetone wash may be used
as the final wash after potassium hydroxide-ethylene glycol
solution is removed from the specimen to improve drying
times.
A3.9 Place the specimen in an oven at 100°C minimum
until the sample is dried (approximately 1 h at 100°C).
A3.10 Cool the filter or crucible to room temperature in a
desiccator. Weigh the specimen in its holder, Mcr, to the nearest
0.0001 g.
A4.3 Place each specimen into a suitable beaker.
A4.4 Add 20 to 25 mL of 40 to 80 % sodium hydroxide
solution to the beaker and heat specimen on a hot plate to 80°C
maximum. Heat used depends on the required heat to digest the
matrix for the system.
A4.5 When the matrix digestion is complete, remove the
beaker from the hot plate and allow to cool.
 D3171 − 15
A4.6 Filter the contents into tared or preweighed, Mc,
sintered glass filters (or crucible with glass filter) under a
vacuum of 50 kPa or better. Wash three times with distilled
water. An acetone wash may be used as the final wash after the
sodium hydroxide is removed from the specimen to improve
drying times.
A5. PROCEDURE E—MATRIX DIGESTION USING HYDROCHLORIC ACID
Warning—Understand the hazards described in Section 9
before working with acids.
A5.1 Weigh each specimen, Mi, to the nearest 0.0001 g.
A5.2 Determine the density of each specimen in accordance
with Test Methods D792 or D1505 if fiber volume percent or
void percent, or both, are required. The preconditioning for
D792 or D1505 specimens is to be in accordance with D3171
Section 12.
A5.3 Place each specimen into a suitable beaker.
A5.4 Add 20 to 25 mL of 5 to 10 % hydrochloric acid
solution to the beaker and heat specimen on a hot plate. Heat
used depends on required heat to digest the matrix for the
system.
A6. PROCEDURE F—MATRIX DIGESTION WITH NITRIC ACID IN A MICROWAVE OVEN
Warning—Understand the hazards described in Section 9
before working with acids.
A6.1 Weigh each specimen, Mi, to the nearest 0.0001 g.
A6.2 Determine the density of each specimen in accordance
with Test Methods D792 or D1505 if fiber volume percent or
void percent, or both, are required. The preconditioning for
D792 or D1505 specimens is to be in accordance with D3171
Section 12.
NOTE A6.1—Specimens may require further dicing or grinding before
digestion. Specimens in the state to be digested should be reweighed after
density determination in this case. Care should be taken that the diced or
ground specimen represents original sample composition.
A6.3 Place each specimen in a specially designed pressure
vessel, which encloses the solution and sample, but allows
pressure release.7 Add at least 30 mL of 70 % nitric acid
solution.
7
The sole source of supply of the apparatus known to the committee at this time
is CEM Corp., P.O. Box 200, Matthews, NC 28104. If you are aware of alternative
suppliers, please provide this information to ASTM International Headquarters.
Your comments will receive careful consideration at a meeting of the responsible
technical committee,1 which you may attend.
10
A4.7 Place the specimen in an oven at 100°C minimum
until the sample is dried (approximately 1 h at 100°C).
A4.8 Cool the filter or crucible to room temperature in a
desiccator. Weigh the specimen in its holder, Mcr, to the nearest
0.0001 g.
A5.5 When the matrix digestion is complete, remove the
beaker from the hot plate and allow to cool.
A5.6 Filter the contents into tared or preweighed, Mc,
sintered glass filters (or crucible with glass filter) under a
vacuum of 17 kPa or better. Wash three times with distilled
water. An acetone wash may be used as the final wash after the
sodium hydroxide is removed from the specimen to improve
drying times.
A5.7 Place the specimen in an oven at 100°C minimum
until the sample is dried (approximately 1 h at 100°C).
A5.8 Cool the filter or crucible to room temperature in a
desiccator. Weigh the specimen in its holder, Mcr, to the nearest
0.0001 g.
A6.4 Place lid on the vessel and attach tubing so that nitric
acid vapor will be off-gassed to release pressure. Set time and
power requirements of the microwave in accordance with the
size of specimen and composite system.
A6.5 The maximum time for digestion should be 30 min.
Shorter times are dependent on the system. The matrix is
considered fully digested if no trace of the reinforcement/
matrix laminate combination remains. Unfortunately, this is
difficult to detect until the specimen has been removed from the
digestion media.
A6.6 Filter the contents into tared or pre-weighed, Mc,
sintered glass filters (or filter-lined crucibles) under a vacuum
of 17 kPa or better. Wash the fiber three times with distilled
water. An acetone wash may be used as the final wash after
nitric acid is removed from the specimen to improve drying
times.
A6.7 Place the specimen in an oven at 100°C minimum
until the sample is dried (approximately 1 h at 100°C).
A6.8 Cool the filter or crucible to room temperature in a
desiccator. Weigh the specimen in its holder, Mcr, to the nearest
0.0001 g.
 D3171 − 15

A7. PROCEDURE G—MATRIX BURNOFF IN A MUFFLE FURNACE

A7.1 Weigh each specimen, Mi, to the nearest 0.0001 g.
A7.2 Determine the density of each specimen in accordance
with Test Methods D792 or D1505 if fiber volume percent or
void percent, or both, are required. The preconditioning for
D792 or D1505 specimens is to be in accordance with D3171
Section 12.
NOTE A7.1—Specimens may require further dicing or grinding before
burn off. Reweigh specimens after machining. Care should be taken that
the diced or ground specimen represents original sample composition.
A7.3 Place each specimen in a desiccated preweighed
crucible, Mc. The crucible should be cleaned by heating to 500
to 600°C or more in a muffle furnace and cooled in a desiccator
before weighing.
A7.4 Place the crucible into a preheated muffle furnace at
500°C or lower depending on the composite system (a tem-
perature below the temperature at which samples will sponta-
neously ignite). Heat to 565 6 30°C, or other temperature
compatible with the composite system, that will burn off the
matrix and leave the reinforcement.
NOTE A7.2—Materials placed in such a hot environment may ignite.
Specimens may be ignited under a controlled heat flame before entrance
into a muffle furnace. If specimens are preignited, the muffle furnace may
be set at the actual burn-off temperature.
A7.5 The maximum time for burn off should be 6 h. Shorter
times are dependent on the system and specimen size. The
matrix is considered combusted if no matrix/reinforcement
block exists. Ash and reinforcement should be the only items
visible.
A7.6 Place the specimen and crucible in a desiccator and
allow to cool to room temperature.
A7.7 Weigh the specimen in its holder, Mcr, to the nearest
0.0001 g.

A8. PROCEDURE H—MATRIX CARBONIZATION IN A NITROGEN-PURGING FURNACE

A8.1 Determine the density of each specimen in accordance
with Test Methods D792 or D1505 if fiber volume percent or
void percent, or both, are required. The preconditioning for
D792 or D1505 specimens is to be in accordance with D3171,
Section 12.
A8.2 Weigh each composite specimen, Mi, to the nearest
0.0001 g.
A8.3 Weigh neat resin specimen (the same resin used as
matrix in the fiber reinforced composite), mi, to the nearest
0.0001 g.
A8.4 Place the composite specimen in a desiccated pre-
weighed crucible, Mc. The crucible shall be cleaned by heating
to 500 to 600°C or more in a furnace and cooled in desiccator
before weighing.
A8.5 Place the neat resin specimen in a desiccated pre-
weighed crucible, mc. The crucible shall be cleaned by heating
to 500 to 600°C or more in a furnace and cooled in desiccator
before weighing.
A8.6 Place the crucibles into a nitrogen-purging furnace and
heat to 560 6 40°C. The minimum time for carbonization shall
be 1 hour at temperature.
A8.7 Cool the crucibles to room temperature in the furnace
with nitrogen still being purged. Check for residue of the neat
resin specimen. If any exists, weigh the residue from the neat
resin specimen in its holder, mcr, to the nearest 0.0001g. If no
residue exists, mcr is equal to mc.
A8.8 Weigh the residue from the composite specimen in its
holder, Mcr, to the nearest 0.0001g.

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