Fingerprinting Toolbox (1)

8/7/2019 Fingerprinting Toolbox (1)

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Chemical

Fingerprinting

Objectives and

Overview


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Basic Problem: Raw materials (polymers, adhesives, cleaners)

meet specifications, but are different enough to cause

manufacturing or flight performance issues, for example:

Multiple cases of silicone contamination on various process materials

from vendor changes in end item materials

Differences from unplanned or unknown vendor process changes,

contamination, or changes at sub-tier suppliers

Lesson Learned: Supplier process changes or contamination can

produce in-spec materials that are subtly (but critically) different

and can cause significant problems with hardware fardownstream

Solution: Fingerprint material to screen important end items and

process materials; provide ongoing assurance that nothing creeps

into processes to surprise at a later date

Challenge: Detecting subtle (but important)

changes in supplier material constituents


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Material Component Team

Multi-function teams define materials to fingerprint and methods

to accomplish

Material team representation may include:

Material Specialist / Material and Process Specialist

Design Engineer

Procurement Quality Engineer

Manufacturing Engineer

Process Control Lab

Research and Development Analytical Laboratories

Quality

Operations Quality Lab (Material Receipt)


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Fingerprint Definition

Key is a chemical fingerprint that can be used to identify a material, todifferentiate it from similar looking materials, or lead to its source

Fingerprinting methods used to characterize materials and processes Following a failure or noncompliance

Ad hoc, reactive, and incomplete generation and storage of data Database scattered over dozens of file cabinets

Few techniques were adopted for receiving inspection/process control

Diagnostic combination of analytical methods for

detailed characterization of a material


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Objectives of Chemical Fingerprinting

Enhanced understanding of material composition

Standardized approach to material evaluation

Develop a comprehensive material characterization database

Reduced probability of unexpected and unrecognized changes

to critical materials and processes

Enhanced ability to detect subtle changes in a material and its

chemical makeup due to factors such as:

Material obsolescence

Ozone depleting compound (ODC) and other environmental issues

Sub-tier supplier changes

Better understand how a material works, ages, degrades, etc.


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TRANSITION PERIOD

Perform current and fingerprintingacceptance testingAccept material using current testing and specification

Evaluate new results periodically Transition when, ready to accept fingerprinting tests

IMPLEMENTATION

Select fingerprint limits Update specification

EVALUATE SIGNATURE

Downselect applicable techniques

Establish method/material variations Set preliminary fingerprinting limits

REVIEW RAW MATERIAL

Review existing data Contact supplier(s) Select analytical instruments Prepare test plans Compile database reference data

Phase IIImplementation

Laboratory Team

Material Team

Material Team

GENERATE TOTAL SIGNATURE

Develop analytical methods Sampling Sample preparation/separation Instrument operation

Determine precision and accuracy Establish quality controls

Document analytical test methods Provide training/transfer to the QA lab

FingerprintingPlan Phase I

Development

Material Team

Material Fingerprinting Approach


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Chemical Fingerprinting

for the Reusable Solid

Rocket Motor (RSRM)at ATK Thiokol


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ATKThiokol uses a comprehensive system to fingerprint

critical materials supporting the RSRM

Extensive instrumentation and capabilities in R&D analytical

laboratories defined optimal fingerprinting methods

RSRM Fingerprinting Data Management Systemmanipulates and stores computerized profiles of materials

Following slides outline techniques and systems used

For additional information, contact

Rick Golde: 435-863-3423, [email protected] - or

Glen Curtis: 435-863-6954, [email protected]

Fingerprinting for RSRM


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RSRM Components Involving Critical Materials

Forward

Center

Center

Aft

CastingSegments

Nozzle Protective Plug

Propellant

Segmented steel case

Movable nozzle

Case-bonded,composite solidpropellant

Elastomeric internalinsulation

Nozzle ablative liner

Nozzle insulator andstructural shell

Clean bonding surfaces

Effective adhesives

ALL RSRM materials and constituents

are critical and need to be monitored


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R&D Analytical

Laboratory

Instrumentationand Capability


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Chemical Analysis

Nuclear magnetic resonance (NMR) (300 and 400 MHz)

Surface analysis Electron spectroscopy for chemical analysis

X-ray photoelectron spectroscopy (ESCA/XPS)

Auger

Secondary ion mass spectrometry (SIMS)

Ion scattering spectrometer (ISS)

RAMAN / Fourier transform infrared (FTIR) / Near infrared (NIR)

Metals analysis Inductively coupled plasma (ICP) emission

ICP-Mass spectrometer (MS)

Atomic absorption/Graphite furnace atomic absorption (AA/GFAA)

X-Ray

Flow injection auto analyzer

Element analysis (carbon, hydrogen, nitrogen, oxygen, sulfur)

Chromatography High-performance liquid chromatography (HPLC) /HPLC-MS

Gas permeation chromatography (GPC)

Gas chromatography (GC) (various detectors)

Gas chromatography - Mass spectrometer (GC/MS)

Ion chromatography (IC)

Classical techniques

Asbestos identification


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Thermal Analysis

Differential scanning calorimetry (DSC)

Microcalorimeter

Accelerating rate calorimeter (ARC)

Adiabatic calorimeter

Thermal mechanical analysis (TMA)

Thermogravimetric analysis (TGA) TGA/Mass spectrometer (MS)

Pyrolysis gas chromatograph / Mass

spectrometer (GC/MS)

Thermal conductivity

Strand burner

Window bomb

Quench bomb

Material compatibility

Specialized instrumentation


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Mechanical Properties Characterization

Mechanical testing equipment Five servo-hydraulic machines

Nine electro-mechanical machines

Two DMA spectrometers

Impact testers

Tensile properties

Dynamic properties

Fracture energy

Hardness

Thermal coefficient of linearexpansion (TCLE)

Volume dilatation

Environmental control

Test rates to 10,000 ipm

Simulation to full-scale article testing

Machining and sample preparation

Aging


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Surface Characterization Systems

Eddy Current

Ultrasonics Fourier transform infrared

SurfMap-II

Thermal Imaging

Sensors Fiber Optic Strain Systems

Mid IR Fiber Optic Chemical Sensing

Piezoelectric Sensors

Acoustic Waveguides

Nondestructive Evaluation


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Fingerprinting

Analysis andDatabase


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RSRM Fingerprinting Data Management

Manual Data

Storage

Automated

Data Storage

Data Storage

Raw Da ta , conve rted GRAM S, and

other f i les are stored on the

se rve r. Quan t i ta t i ve da ta and

m a t e r i a l d e f i n i t i o n i n f o rm a t i o n i s

stored in Naut i lus.

Quantitative Data

Nautilus Lims Sy stem

MS Word or

Powerpo in tMerck IndexChemDraw

Excel

Spreadsheets

S c a n n e d I m a g e s

Fingerprinting Data Manipulation & Storage

PresentationManager

Fingerprinting V iew erFile Stora ge

Lan Se rve r

Au tomated

GRAMS

Converson

Fingerprint ing

Data LoaderLab Equipme nt

Manual

GRAMS

ConversionData i s manua l l y

o r a u t o m a t i c a l l y l o a d e d

in to the app rop ri a te

storage area.


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Database Viewer Features

Executive View Material overview, reference documents,

data examples

Method Information Chemical characterization methods

Component Information Trend analysis and visualization of key analytes

Method Quality Control Trend analysis of QC parameters

View Comparison Direct graphical overlay of raw spectroscopic

and chromatographic data

Lab Notes


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EPDM (ethylene-propylene-diene monomer) Usage in the booster motor

Material Example: Neoprene in EPDM Insulation


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Executive Screen for Neoprene FB


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Method Information Screen


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Component Info: Analyze Trends


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Method QC: Duplicate Gas Permeation

Chromatography Analysis Trends


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View Comparison: Fourier Transform Infrared Data


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0

r

595

r

714

r

764

r

835

r

19

r

185

r

168

r

331

r

0.010

0.015

0.020

0.025

0.030

0.035

0.040

0.045

0.050

0.055

0.060

0.065

0.070

0.075

0.080

0.085

r

1480149015001510152015301540

-1

Analysis Details: Fourier Transform

Infrared Spectra From Aging Study


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Fingerprinting

Successes andSummary


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Neoprene FB Secondary polymer used as a component in EPDM formulations

(material no longer produced)

Fingerprinting showed that under proper storage conditions - NeopreneFB could be stored over10 years and still meet specification

Storage at40rF, low humidity, and minimal light

Stockpiled 100,000 lbs till new EPDM formulation can be qualified

Test methods developed to ensure material is well within specification

Viscosity measurement performed as a check at the vendors storage site,while the GPC and FTIR analyses confirm the molecular weight distributionand the chemical composition

Similar program experienced solvating problem with gum stock forcarbon fiber EPDM

Fingerprinting knowledge allowed immediate identification of the problem

Corrective action given on controlling Neoprene FB

Material Fingerprinting Successes


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Brulin 1990 GD Environment-friendly replacement for methyl chloroform vapor

degreasing

Water-based solvent used with spray-in-air technology

Several issues developed with material during certification

Material received with insoluble material in drums Material received with lower than expected pH

Vendor requested site visit by primes chemist

Knowledge from fingerprinting provided information to stabilize product

through small changes in use of de-ionized water, mixing steps and cycles

Use of hydrated silicates

Recommendation for additive to spray in air baths

Increased useable bath life from 8 to 90 days

Knowledge from fingerprinting effort provided suggestion for corrosion

inhibitor rinse cycle (new inhibitor currently qualified)


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Carbon Cloth Phenolic (CCP)

Carbon cloth prepreg phenolic resin used to fabric nozzle

components

Test methods developed to enhance characterization of

phenolic resin Detailed analysis of CCP prepreg enables monitoring of

compositional factors that can affect material behavior

ITGA (Isothermal Gravimetric Analysis) - new method to

quickly determine adequate carbonization of cloth

Test discriminates material propensity for pocketing Eddy current method developed to measure cloth

carbonization in cloth and prepreg materials


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HD2 grease from new plant verified

Conoco tried new formulation, but reverted to original catalyst

after fingerprinting confirmed it gave most consistent result

D-limonene containing solvents removed from use on

uncured rubber after testing confirmed degradation of curesystem

BHT identified as a minor additive to inhibit d-limonene

polymerization in PF degreaser

Chemlok aging studies based on FTIR suggests that one

resin component shows significant degradation in less thanone year after exposure to ambient air


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General Benefits of Fingerprinting

More fundamental understanding of critical materials

Provide baseline chemical profile of materials in use

Lot-to-lot consistency can be monitored and changes flagged

Material changes can be traced to their source

Acceptance testing for small supplier who cannot afford lab

support

Instills technical ownership for critical materials

Enhances re-qualification of changes at vendor or production

Improved vendor relationship through data sharing

Database available for failure analyses

Fingerprinting Toolbox (1)

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