Additives Analysis for Polymers and Plastics
in Toray Research Center
Additives contained in polymers, plastics, which is one of the items analysis is required widely.
Based on the accumulated preparation know-how or analytical skills in , Toray Research Center
we shall provide advanced services for identifying unknown additives.
Objective（Analytical Approach）

Choice of Analytical Method
Sample information

Specification of unknown
Compounds , Analysis ofdegradation products

Additive content(Quantitation)

Correlation analysis among
physicality, performance
Investigation of manufacturing
loss

Additives

Polymer Species・Sample amount・Sampling position

Additive composition(Qualification)（Stabilizer, Function imparting agent,Reactant, e.g.）

Solvent solubility

Choice of Measurement and evaluation

Choice of Preparation method

Other measurements

Additive Mw

Solvent‐soluble

High

Separation of additives from Polymers
With Dissolution and re‐precipitation
Solvent‐insoluble
Solvent extraction

104

2000

Chromatographic
Fractionation,
If necessary

500

MALDI‐MSPy GC/MS, SEC, HPLC
HPLC(UV,ELSD,CAD)
LC/MS

Detection of Characteristicelements, which is included in additives

NMR

Quantitation of specific elements
Detection of active HALS
(Hindered amine stabilizer )GC, GC/MS※Quantitative values should be handledwith care, because it is difficult to extractthe entire amount in sample.

LowsmallESR

large Content

Suggested Analysis Flow Examples
and Results

SampleQualification of anti‐oxidant, UV‐absorbent● LC/PDA, HR‐LC/MS, GC/MS

Qualification of HALS including high‐molecular types●Py GC/MS

CH3

CH3 H CH3
CH3 H CH3N
N
CH3 CH3CH3NCH3N

CH3 H CH3NCH3Preparation

Separation withoptimization ofconditions

HN (CH2)6（Separation of additives from polymers)

CH3Crushing, centrifugal separation, drying,solvent extraction etc.

CH3(CH2)6NStructure estimationfrom thermolysis
productsNNNH
C8H17NH

CH3N
CH3 H CH3Chimassorb944

CH3 H CH3N
CH3

CH3 H CH3
CH3 H CH3NN
CH3
CH3 CH3CH3N

Step1

H N (CH2)6Qualification

HPLC chromatogram
UV spectrum
skeletal structure

High‐Resolution MS spectrum
MS/MS spectrum

Spectroscopic
Analysis

Formula, Partial structure

Identification with additive spectra databaseaccumulated in Toray Research Center

Database
SearchIdentification

Step2Quantitation
Quantitation of Surfactants , HALS, whichhave a molecular weight distribution

High‐sensitive detection●LC/CAD, LC/ELSD, LC/MS/MS

It is important
to apply multiple
measurements forcomplementary analysis

Examples of Analytical Results
Species

CH3CH3N (CH2)6N
CH3 H CH3N

HNNH
C8 H17

CH3CH3NCH3 H CH3Reaction Py GC/MS result（TICC）●MALDI‐MS of GPC fractions, HR‐LC/MS/MS
Possible to identify high‐molecular types , polymer‐
binding additives

Quantitative analysis of anti‐oxidant●GC, GC/MS/MS
Scan

GC/MS

GC/MS/MS

High‐sensitive
detection withMS/MS
optimization

BHT
10ng/mL●LC/UV, LC/CAD, LC/ELSD, LC/MS/MSClassification of Additives
Ｐｒｉｍａｒｙ ａｎｔｉｏｘｉｄａｎｔ
Stabilizer
Secondarｙ ａｎｔｉｏｘｉｄａｎｔ

NNNminPhenol‐based
phosphoric acid‐based , Sulfur‐based
PP, PE, PS, ABS
Benzotriazole‐based,
Benzophenone‐based, Polymer‐
PC, PET, PBT, PA Function UV absorbent
binding type
Gum（SBR,EPDM） impartingN‐H type, N‐CH3 type、NO‐alkyl type, High‐molecular, e.g.
agent HALS(Hindered amine light stabilizer) type
Others Surfactants, Polymerization initiator or inhibitor, Flame retardants, Antibacterial agent, e.g.

Examples of analytical results
Irganox1010 0.5%, Quinone methide 0.01%
PEP36 0.1%, DLTDP 0.2%
Tinuvin 326 0.2%
Chimassorb944 0.2%

PEG 0.1%, MEHQ 0.02%
P01452有機分析化学第２研究室20160408-2