T1200017 V0

LASER INTERFEROMETER GRAVITATIONAL WAVE OBSERVATORY

TEST PROCEDURET1200017-

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Glove, Wiper and Solvent Interaction Test

AUTHOR(S) DATE Document Change Notice, Release or ApprovalPatrick Murphy 01/10/2012 see LIGO DCC record Status

1 Objective

This document determines if a reaction if any, exists between PPE latex gloves Ansell Accutech 91-300C, cleanroom use wipers ITW Texwipe TX1010, Berkshire Microseal Supersorb , ITW Texwipe Vertex TX22 and Reagent grade Acetone solvent through qualitative FTIR. Better tests are available to make Quantitative determinations of NVR(Non-Volatile Residues) present after mechanical agitation at 100RPM and 5 minute dwell. Would need a balance with 0.0000 gram measurement capability to calculate by mass the NVR of the glove, wiper, solvent system.

2 Applicable DocumentsReference DocumentsITW Test Method TM1 Matter Extractable from Wipers and Other MaterialsITW Test Method TM14 The Determination of the Surface Resistivity of Fabrics and Other Thin Flat MaterialsITW Test Method TM18 The Determination of Ions in Wipers by Ion ChromatographyITW Test Method TM22 Particle Release from Wipers and Other Materials Under Conditions of Moderate Mechanical StressBerkshire Test Methods IEST-RP-CC04.3 Evaluating Wiping Materials Used in CleanroomsBerkshire Wiper Tests for Cleanliness, Sorbency and PurityJournal of IEST Nov/Dec 1998 Comprehensive Particle and Fiber Testing for Cleanroom WipersAuthors: Himansu R. Bhattacharjee and Steven J. PaleyMicro Feb 1997 Evaluating sample preparation techniques for Cleanroom Wiper TestingAuthors: Himansu R. Bhattacharjee and Steven J. PaleyAuthor: Brian Smith, Fundamental FTIR Glossary, Retrieved fromhttp://www.spectros1.com/pdf/Fund_FTIR_Glossary.pdf Note :( All Reference documents must be procured on individual and copyrighted basis.)

3 Materials and EquipmentList of required consumables and equipment:

Frock, Bouffant Cap, Mask, Boot covers, gloves **See Contamination Control Appendix in DCC**

Cleanroom environment and Fumehood minimum

Ansell 91-300C Latex gloves, powder free Mfr: Ansell Products

Vectra Alpha 10 Wiper Sealed Borders P/N TX1010 Mfr: ITW Texwipe

Vectra Alpha 10 Wiper Sealed Borders P/N TX1012 Mfr: ITW Texwipe

Vertex Laser Sealed Edge Wipers P/N TX22 Mfr: ITW Texwipe

Microseal Supersorb Class 10 100% Polyester Wipers Mfr: Berkshire

LIGO Form T1200017-v0

https://dcc.ligo.org/cgi-bin/private/DocDB/ShowDocument?docid=78512




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List of required consumables and equipment continued:

Methanol Reagent Grade (ACS)

Isopropyl Alcohol Reagent Grade (ACS)

Acetone Reagent Grade (ACS)

Pyrex Dish and cover

500ml Beaker

Stainless Steel Tweezers

Lab-Line Instruments Orbital Shaker Model 3527

5 Gallon Safety Can for waste solvents

Safety Can for solvent soaked rags

Glass Qorpak 30ml / 1 oz bottles with Teflon lined caps






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4 Definitions

4.1 Absorbance - units used to measure the amount of infrared radiation absorbed by a sample. Absorbance is commonly used as the Y axis unit in infrared spectra. Absorbance is defined by Beer's law, and is linearly proportional to concentration. This is why spectra plotted in absorbance units should be used in quantitative analysis.

4.2 ATR - stands for Attenuated Total Reflectance, and is a reflectance sampling technique. In ATR, infrared radiation impinges on a prism of infrared transparent material of high refractive index. Because of internal reflectance, the light reflects off the surface of the crystal at least once before leaving it. The infrared radiation sets up an evanescent wave which penetrates a small distance above and below the crystal surface. Samples brought into contact with the surface will absorb the evanescent wave giving rise to an infrared spectrum. This sampling technique is useful for liquids, polymer films, and semisolids.

4.3 Background Spectrum - a single beam spectrum acquired with no sample in the infrared beam. The purpose of a background spectrum is to measure the contribution of the instrument and environment to the spectrum. These effects are removed from a sample spectrum by rationg the sample single beam spectrum to the background spectrum.

4.4 Baseline Correction - a spectral manipulation technique used to correct spectra with sloped or curving baselines. The user must draw a function parallel to the baseline, then this function is subtracted from the spectrum.

4.5 Beer's Law - the equation that relates the absorbance of a sample to its concentration. Its form is

A = εlc where the A is stands for absorbance, ε for absorptivity, l is for pathlength, and c is for concentration. Beer's law is the equation used in FTIR quantitative analysis to perform calibrations and to predict unknown concentrations.

4.6 Calibration - the process in quantitative analysis by which the peak heights and areas in a spectrum

are correlated with the concentrations of analytes in standards. After calibration, the concentration of the analyte in unknown samples can be predicted.

4.7 Calibration Curve - a plot of absorbance versus concentration used in a calibration. If the plot is

linear, it means Beer's law has been followed, and that the plot can be used to predict the concentration of unknown samples.

4.8 Capillary Thin Film - a transmission sampling technique used to obtain spectra of liquids. Typically, a drop of liquid is placed between two KBr windows, and the windows and sample are placed directly into the infrared beam. The capillary action of the liquid holds the two windows together, hence the name of the technique.

4.9 Cast Films - a transmission sampling technique used to analyze polymer films. The polymer is dissolved in a solvent, and the solution is evaporated onto a KBr window giving a polymer film. The window/film combination is then placed directly in the infrared beam.






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4.10 Chromatograph: A device used to separate complex mixtures into their components. Chromatographs measure chromatograms, which are plots of detector response versus time. Chromatographs can be used to quantify the concentration of molecules in a sample.

4.11 Coadding: The process of adding interferograms together to achieve an improvement in signal-to-noise ratio.

4.10 Cleanliness: is both the abstract state of being clean and free from dirt, and the process of achieving and maintaining that state.

4.11 Evanescent Wave - in ATR, the standing wave of radiation set up in the ATR crystal. The evanescent wave penetrates beyond the crystal surface into any sample brought into contact with the surface. As a result, the infrared spectrum of the sample can be obtained.

4.12 Fourier Transform - the calculation performed on an interferogram to turn it into an infrared spectrum. The calculation involves a mathematical integral.

4.14 FTIR : a method of obtaining infrared spectra by first measuring the interferogram of the sample using an interferometer, then performing a Fourier transform on the interferogram to obtain the spectrum.

4.15 Full Spectrum Search: in library searching, the use of entire spectra when comparing unknown and library spectra. The advantage of this method is that the use of all the spectral data points gives a more accurate comparison.

4.16 Gram-Schmidt Chromatogram - in GC-FTIR, a plot of total infrared absorbance versus time. This chromatogram is used to determine how many sample components were detected by the FTIR.

4.17 Hyphenated Techniques - when an FTIR is interfaced to another instrument that also performs chemical or physical analyses, a hyphenated technique is born. The name derives from the fact that the new technique is usually abbreviated with a hyphen and the letter FTIR, such as GC-FTIR. By interfacing FTIRs to other instruments, more information about a sample can be obtained more quickly than using the two instruments to analyze the sample separately.

4.18 Orbital Shaker: A solid state speed controller allows for variable speeds between 40 and 400 orbits per minute. An electronic tachometer displays the shaker speed. A triple eccentric shaker mechanism, powered by a 1/15 HP motor, imparts a ¾" circular motion to the shaker platform. The drive rotates on nine permanently lubricated ball bearings. The entire drive is isolated from the shaker chamber, thus preventing damage to the mechanism should glassware accidentally break in the chamber. A timer allows for continuous operation or timed shaking up to 60 minutes. An acrylic cover allows for undisturbed viewing of the entire shaking chamber.

4.19 NVR: Non-Volatile Residue






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4.20 Reference Spectrum - in spectral subtraction, the spectrum of a substance that is subtracted from the spectrum of a mixture (sample spectrum). Often, the reference spectrum is of a solvent.

4.21 Reflectance Sampling: A method of obtaining infrared spectra by bouncing the infrared beam off of

the sample..

4.22 Reflection-Absorption: A reflection sampling technique used on thin films coated on shiny metal surfaces. The infrared beam passes through the film, reflects off the metal, then passes through the film a second time before reaching the detector. This technique is also known as "double-transmission".

4.23 Resolution: A measure of how well an infrared spectrometer can distinguish spectral features that are close together. For instance, if two features are 4 cm-1 apart and can be discerned easily, the spectrum is said to be at least 4 cm-1 resolution. Resolution in FTIR is determined by optical path difference.

4.24 Reststrahlen - derivative shaped spectral features that occasionally appear in specular reflectance spectra. Restsrahlen is caused by how a sample's refractive index changes in the vicinity of an absorbance band. The Kramers-Kronig transform can be used to remove restsrahlen from spectra.

4.25 Sample Single Beam Spectrum: The single beam spectrum obtained with a sample in the infrared beam. These spectra are typically ratioed against background spectra to obtain absorbance or transmittance spectra.

4.26 Sample Spectrum: In spectral subtraction, the spectrum of a mixture from which the reference spectrum is subtracted.

4.27 Solute: The component of a solution that does not change its state in forming the solution. 4.28 Sorbency: The ability of a sorbent material to gather on a surface either by absorption, adsorption,

or a combination of the two processes.

4.29






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5 Solvent, Wiper, and Glove Interaction TestingAll wipers were tested with the same LOT# Ansell Latex Powder free 91-300C glove Size 8.0:

I. Baseline Specimen Test vessel and Acetone ACS Grade

II. Ansell 91-300C and ITW Vectra Alpha TX1010 Sealed Border Wiper

III. Ansell 91-300C and ITW Vectra Alpha TX1012 Sealed Border Wiper

IV. Ansell 91-300C and ITW Vertex TX22 Laser Sealed Border Wiper

V. Ansell 91-300C and Berkshire Microseal Supersorb Class 10 Wiper

5.1 Test Matrix

91-300C GloveTX1012 Wiper30 ml sample

1) LOT# 10101711EV2) 11.2 11.6

FTIR Sample30 ml Acetone

ACS gradeGlove and Wipers

InformationInitial

Glove (grams)Initial

Wiper (grams)Final

Wiper (grams)

1) 91-300C Glove2) TX1010 Wiper

30 ml sample1) LOT# 10101711EV2) Code 11-471566 10.6 6.1 6.2*

Baseline Acetone30 ml sample from 500ml NA NA NA

91-300C GloveTX22 Wiper

30 ml sample1) LOT# 10101711EV

2) LOT# F141AD 11.1 10 10.2*

91-300C GloveMicroSeal Wiper

30 ml sample1) LOT# 10101711EV

2) LOT# 0785813 11.1 12.9 13

Final Glove (grams)

NA

12.1*

11.2

11.1

11.2

NA

11.6

Note: The purpose of this testing was to see if anything is leached into the solvent during cleaning from the PPE(gloves) and cleaning materials(wipers and solvents) that could leave a residue.






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6 Test Method Cleaned fume-hood with Isopropyl Alcohol and TX1010 wipers

Lined with UHV Foil to create clean work surface see Image 13

Triple rinsed sample bottles in IPA, Methanol and Acetone see Image 7






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Triple rinsed Pyrex pan and lid in IPA, Methanol and Acetone see Image 2

Set Orbital Shaker to 100 RPM, and a 5 minute dwell






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Weigh the glove and record the initial weight Weigh the wiper and record the initial weight Measure 500ml of Acetone ACS grade Place glove, wiper and 500 ml of solvent into Pyrex Pan

and cover lid Transfer to Orbital shaker set at 100 rpm and 5 minute

dwell Start timer Upon completion of 5 minute dwell, use Stainless steel

tweezers to remove the wiper and glove and allow to dry under fume hood on individual pieces of UHV Aluminum Foil

Transfer contents of Pyrex Pan into 500ml beaker and fill 30ml Qorpak bottle to line and place Teflon lined Green cap on and seal with proper identification

Transfer balance 430 ml into waste container When wiper and glove have dried record final weights Request FTIR testing priority from Bob Taylor Send FTIR samples to [email protected] Update this document with pending results




mailto:[email protected]



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Appendix






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Annex AImages of setup and equipment

Image 1 Orbital Shaker






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Image 2 Pyrex Pan in Fumehood

Image 3 Microseal Supersorb Wiper






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Image 4 Vertex Laser Edge Wipers






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Image 5 Alpha 10 Synthetic Wiper






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Image 6 Vectra Alpha 10 Sealed Border Wiper






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Image 7 Qorpak Sample Bottles post triple rinses






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Image 8 Ansell 91-300C Powder-free Latex Gloves






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Image 9 Acetone ACS Grade






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Image 10 Methanol ACS Grade






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Image 11 Isopropyl Alcohol ACs Grade






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Image 12 Qorpak Teflon Lined Lids






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Image 13 UHV Aluminum Foil


