Tiêu chuẩn iso 17881 1 2016

© ISO 2016 Textiles — Determination of certain flame retardants — Part 1 Brominated flame retardants Textiles — Détermination de certains retardateurs de flamme — Partie 1 Retardateurs de flamme bromé[.]

Tex tiles — Determination ofcertain

Part 1:

Te xtile s — Déte mination de c rtains r tardateurs de flamme —

Partie 1: Retardateurs de flamme bromés

Fir t edition

2 16-0 -0

Refer ence n mb r

ISO 178 1-1:2 16(E)

COPYRIGHT PROTECTED DOCUMENT

© ISO 2016, P blshed in Sw itz rlan

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the r eq eser

ISO c pyrig ht ofic

C de Blan on et 8 • C 4 1

CH-1 14 Vernier, Geneva, Sw itzerlan

F reword i v

1 Sc ope 1

2 Principle 1

3 Re g ents 1

4 A pparatus 2

5 Proc ed re .2

5.1 Pr eparation of s an ar d solutions 2

5.1.1 Stock s an ar d solution 2

5.1.2 Inte nal s an ar d solution 2

5.1.3 Wor king solution 3

5.2 Pr eparation of tes spe imen 3

5.3 Ultrasonic wa veex tr action 3

5.4 Flamer etar dants dete mination 3

6 Calculation 3

7 Test rep r t 4

A nne x A (informative)Test parameter s b GC-MS 5

A nne x B (informative)Ro nd Ro in test 7

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The committ ee r sp nsible for thisdocument is ISO/TC3 , Tex ties

ISO 1 88 consis s of the folowing p rt , u de the g ene al title Tex ties — Dete min tio o c ertain

flame r tarda ts:

— Part 1: B romin ted flame r tarda ts

— Part 2 : Ph s ph rus flame r tarda ts

Tex tiles — Determination ofc ertain flame retardants —

Part 1:

WARNING — This Internatio al Standard cal s for the use of substances and/or proced res

that may be injurio s to he lth if adeq ate precautio s are n t taken It refer o ly to technical

suitabi ity and d es not absolve the use from le al obl g tio s relating to he lth and safety at

any stag e It has be n as umed in the draf ing of this Internatio al Standard that the ex ecution

of its pro isio s is entrusted to ap ro riately qual fied and ex erienced peo le

This p rt of ISO 1 8 1 spe if ies a t es method for det ermining some brominat ed flame r tardant in

t exties b g s chromat ogra hy – mas spe trometry (GC-MS)

The method isa plca le t o al kinds of t extie prod ct

The flame r tardant ar extract ed from t extie spe imen b ultrasonic gene ator with toluene The flame

r tardant in the spe imen ar identified b GC-MS an q antified b using internal s an ard method

Unles othe wise spe if ied, use only r ag ent of r co niz d analytical grade

3.1 Mo o r omo iphenyl (Mo oBB), CAS no 2 5 -0 -5

3.2 Dibromo iphenyl (DiBB), CASno 5 42 -77-2

3.3 Tr ibr omo iphenyl (Tr iBB), CASno 5 08 -34-1

3.4 Tetrabromo iphenyl (TetraBB), CAS no 6 04 -24-8

3.5 P entabromo-1,1’-biphenyl (P entaBB), CAS no 5 0 0-3 -6

3.6 He xabr omo iphenyl (HexaBB), CAS no 6 04 -2 -0

3.7 Heptabromo-1,1’-biphenyl (HeptaBB), CAS no 8 7 0-0 -5

3.8 Octabromo iphenyl (OctaBB), CAS no 6 8 9-0 -3

3.9 No abromobip enyl (No aBB), CAS no 6 2 8-6 -2

3.10 Decabromo iphenyl (DecaBB), CAS no 1 6 4-0 -6

3.11 Tetrabromo iphenylether (TetraBDE), CASno 5436-43-1

3.12 Pentabromodip enylether (P entaBDE), CAS no.3 5 4-8 -9.

3.13 Hexabromo iphenylethe (HexaBDE), CASno 2 7 2 -1 -4

3.14 Heptabr omodiphenylether (HeptaBDE), CAS no 2 7 22-1 -5

3.15 Octabromo iphenylether (OctaBDE), CASno 3 75 3-72-1

3.16 Decabr omo iphenylethe (DecaBDE), CAS no 1 6 -1 -5

3.17 He xabr omocyclo o ecane (HBCDD), CAS no 2 6 7-9 -4

3.18 Decachlorobiphenyl, CASno.2 5 -24-3, inte nal s an ar d (IS)

3.19 Toluene

NOTE Since brominated flame retardants have man isomer , this method might not cover al of them

Det ermination of the isomer of flame retardants in Clause 3 can refer to this method ac ording to the principle

4 A pparatus

4.1 Gas chromatog raphy – mas spectr ometr y (GC-MS)

4.2 Ultraso ic g enerator, w ith a fr eq ency from 3 kHz to 45 kHz

4.3 E aporator devic e, with wate b th at 5 °C

4.4 Brown glas vial, 40 ml with tight closur e

4.5 Flask, 1 0 ml

4.6 Fitration membrane, 0,45 µm

4.7 Balanc e, an ac ur acy of 0,1 mg

5.1 Preparation of standard solutions

5.1.1 Stock standard solution

Pr p r 1 0 0 µg ml of st ock s andard solutions with individ al flame r tardant (3.1 t o 3.1 ) an

int ernal s an ard (3.1 ) in t oluene (3.1 )

Some comme cial r fe enc mat erial solutions ma be a ai a le in a dife ent solvent

5.1.2 Inter nal standard solutio

Pr p r 1 µg/ ml s an ard solution of de achloro ipheny l in t oluene

5.1.3 Wor king solutio

Pr p r an admixtur working solution of 1 flame r tardant in int ernal s an ard solution (5.1.2)an

diut e it t o a se ies of suita le conc ntrations depen ing on t es ne ds S le t at leas five di utions of

the calbration set t o c eat e calbration curve an pe form GC-MS analy sis

5.2 Preparation of test specimen

Pr p r a r pr sentative t es spe imen of the sample Cut it int o smal pie es an weigh (1,0 ± 0,0 ) g

of the pie es with a b lanc (4.7)

5.3 Ultrasonic wave ex traction

Put the pie es in a vial with tight closur (4.4) and ad 2 ml of toluene Plac the vial in an ultrasonic

gene ator (4.2) an extract the pie es for 3 min at ro m tempe atur Fite and trans e the

extract into 1 0 ml flask (4.5) Ad 1 ml of toluene to the r sid e in the vial and plac the vial in

the ultrasonic gene ator to extract the r sid e for 1 min at ro m tempe atur Fi te an me ge the

extract into the flask (4.5)

Ev porat e theextract t o near drynes b ev porat or devic (4.3) A dd 2 ml of int ernal s an ard solution

(5.1.2) t o dis olve the r sid e an then f ilt er b f iltration membrane (4.6) The f iltrat e is r ady for

det ermination of flamer tardant

5.4 Flame retardants deter mination

Det ermine the flame r tardant in the solution (5.3) b GC-MS(4.1) The t es p ramet ers b GC-MS ar

given in An ex A asan ex mple R un a blank t o control contamination

When the flame r tardant level is ve y low, it is ne es ary t o inc ease the mas of the pie es in orde t o

r ach at leas thr e timesthe det ection lmit

When the flame r tardant level is bey n the lnear det ect or r sp nse rang e of the eq ipment, it is

ne es ary t o diut e the spe imen lq id pro e ly

6 Calculation

Quantify the conc ntration of each flame r tardant b using the calbration curve The cont ent of each

flame r tardant is ex r s ed b the mas ratio of flame r tardant t o t es spe imen, in μg g C lculat e

the r sult b using F ormula (1)

X

m

i

i

=

0

(1)

w he e

X

i

is thecont ent of the flame r tardant, i, in the t extie spe imen, in μg g;

C

i

is theconc ntration of the flame r tardant, i, in the spe imen solution, in μg ml;

C

0

is theconc ntration of the flame r tardant, i, in the blank solution, in μg ml;

V is thef inal v lumeof thespe imen solution, in ml;

m is themas of the t es spe imen, in g

7 Test repor t

The t es r p rt shal inclu e the fol owing information:

a) a r fe enc t o this p rt of ISO 1 88 , i.e ISO 1 8 1-1:2 1 ;

b) al detai s ne es ary for identif ication of the sample t est ed;

c) thecont ent of each flame r tardan

d) any deviation from the proc d r spe ified

A nne x A

(informative)

Test parameter s by GC-MS

A 1 Instrument parameters

As the ins rumental eq ipment of the la orat ories ma v ry, no g ene al y a plca le paramet ers can be

pro ided for chromat ogra hic analy ses The folowing p ramet ers ha e be n foun suc es ful y

a) Ca i ary column: VF-5ht, length 1 m, inside diamet er 0,2 mm,

f ilm thick es 0,1μm or eq iv len

b) Tempe atur pro ramme: 1 0 °C for 2 min, 1 0°C t o 3 0 °C (2 °C min), 3 0°C for 5 min;

c) Inje t or t empe atur : 2 0°C;

d) Trans e lne t empe atur : 3 0°C;

e) Car ie g s: Helum with a purity of no les than 9 , 99 % delve ed at

1,5 ml/min;

h) Det ection mode: S le t ed ion monit or det ection;

i) Inje t or syst em: Spl tles , splt at 1 min;

A 2 T ypical ions and detection l mit

Ty ical ions an det ection l mit or flame r tardant ar shown in Ta le A.1

Table A.1 — Typical ions and detectio lmit

T pical ions/amu Det ection limit

(μg g) Targ t ion Targ t ion

No Flame retardant

T pical ions/amu Detection limit

(μg g) Targ t ion Targ t ion

Table A.1 (c ontin ed)

A nne x B

(informative)

The R ou d R obin t es was car ied out b f ive t extie la orat ories in China

A t otal of nine samples we e pr p r d, thr e from cott on wo en fa rics (no.1 t o 3), thr e from

p lyest er woven fa rics (no.4 t o 6), an thr e from 5 cott on/ 0 p lyest er wo en fa rics (no.7 t o 9)

each containing six flame r tardant , i.e DiB , PentaBB, De aBB, PentaBDE, De aBDE, an HBCDD

The thr e samples from each fa ric we e at thr e conc ntration levels of 5 mg kg, 2 0 mg kg, an

5 0mg kg Thr e t es spe imens from each sample we e t est ed in each la orat ory

The r sult of the Roun R obin t es ar shown in Ta le B.1

Table B.1 — Results of the Round Robin test

Sample

no

Subs anc

E pe t ed

v lue

(mg/kg)

Mean

(mg/kg)

R ecovery

(%)

R epeata i ity R eprod cibi ity

S

r

r

R (mg/kg) CV

R (%)

1

2

3

4

Sample

no

Subs anc

E pe t ed

v lue

(mg/kg)

Mean

(mg/kg)

R eco e y

(%)

R epeata i ity R eprod cibi ity

S

r

r

R (mg/kg) CV

R (%)

5

6

7

8

9

Table B.1 (c ontin ed)