### ~r---~-------------------------------------------------------------------------------~

N 

# ANY

# SAl\l\1IZED~ S? Form Approved. O.M.B. No. 2070-0012. Approval Expires 10-31-96.

### ~,~4MENCY**US~ONLY** 

### U. S. ENVIRONMENTALPROTECTION AGENCY DateofreceipC' ,,' 

# PREMANUFACTURE NOTICE 

# &EPA rn 39 .' 

## ..

# ,­ FOR NEW CHEMICALSUBSTANCES**;::~** \\ h(,11 

### DOCUMENT CONTROL OFFICER OFFICE OF POLLUTION PREVENTION AND TOXIC SUBSTANCES, 7407 Cllll1pl('[('d s('nd this 

### U.S. E.P.A. 401 M STREET, SW form III 

### WASHINGTON, D.C. 20460 Enterthe total numberofpages in the Premanufacture Notice 

# GENERALINSTRUCTIONS

·Youmust provide allinformation requested in this form to the extent thatitis known to or reasonably ascertainable by you. Make reasonable estimates ifyou do not have actualdata• •Before you complete this form, you should read the "InstructionsManual forPremanufacture Notification" (the Instructions Manual is available from theToxic Substances Control Act(TSCA) Information Service by calling202-554-1404, orfadng 202-554-5603). ·Ifa userfee bas been remitted for this notice (40 CFR 700.45), indicate in the boxes above theTS-userfee identification numberyou have generated. Remember,youruser fee ID number mustalso appearon yourcorrespondingfee remittance, which is sentto: EPA, HQ Accounting Operations Branch (PM-266), P.O. 360399M, Pittsburgh, PA 15251-5399, Attn: TSCA UserFee. Part I-GENERALINFORMAnON You mustprovidethe currently correctChemicalAbstracts (CA) Nameofthe new chemical substance, even ifyou claim theidentity as confidential. You may authorize anotherperson to submitchemicalidentity information foryou, but yoursubmissionwill notbecomplete and review will notbegin until EPA receives this information_ A letterinsupport ofyour submission should referenceyour TS user fee indentification number. You must submit an original and two copies ohhis notice including all test data. Ifyou claimed any information as confidential, a single sanitized copy must also besubmitted. Part II-HUMANEXPOSURE AND ENVIRONMENTAL RELEASE Ifthereareseveral manufacture, processing, oruseoperationsto be described in Part 11, sections A and B ofthis notice, reproduce thesections as needed. Part III-LISTOF ATTACHMENTS Attach additional sheets ifthereis notenough spaceto answera question fully. Label each continuation sheet with the corresponding section heading. In Part III,list these attachments, any testdata orother data and any optional informationincluded in thenotice. OPTIONAL INFORMATION You may includeany information that you wnatEPAto consider in evaluating tbenew substance. On page II ofthi!form, space has been provided for you to describe P11l1ution prevention and recycling information you may have regarding tlie new !IIIbstance. So-called "binding" boxes are included throughout this form foryou to indicate your willingness to bebound tocertain statements you makein this notice, such as use, Jlroduction volume, protectiveequipment.
.. This option is intended to reduce delays that routinely accompany the development ofconsentorders or Significant New Use Rules. Exceptin the case ofexemptionapplications (such as TMEA, LVE, LOREX) wherecertain information provided in such notification is bindingon thesubmitterwhen the Agency approves the exemption application, checking a binding box in this noticedm.n!tt by itselfprohibitthesubmitter from laterdeviatingfrom the information (exceptchemical identity) reported in theform.
CONFIDENTIALITY CLAIMS You may claim any information in this notice as conrldential. To assert a claim on the form, mark (X) theconfidential box nextto the information thatyou claim as conrldential. To assert a claim in an attachment, circleorbracket the information you claim as confidential. I fyou claim informationin the potice as confideptialyou must nrovide a sapitized version ofthepotice. ipcluding attachments), Foradditional instructions on claiming information as confidential, read theInstructions Manual. Mark(X) ifany information in this notice is claimed asconfidential TESTDATA AND OTHER DATA You are required to submitall testdata in yourpossession orcontrol and to provide a description ofall otherdata known to Or reasonably ascertainable byyou, ifthesedata are related to tbe health and environmental effects ofthe manufacture, processing, distribution in commerce, use, ordisposal ofthe new chemical substance. Standard literaturecitations maybe submitted for datain theopen scientific literature. Completetest data (written in English), not summaries ofdata. must be submitted ifthevdo notanpearintheonenliterature, You should clearlyidentify whethertestdatais on thesubstanceoron an analog. Also, the chemical composition ofthe tested materialshould be characterized. Following are examples oftestdata and otherdata. Data should be submitted according to the requirements of§720.50 ofthe Premanufacture Notification Rule (40 CFR Part 720). TestData (Check Below any included in this notice)
• Environmentalfatedata 

# 0 Yes • OtherData 

# 0 Yes
• Health effects data 

# 0 Yes Risk assesments
• Environmental effects data 

# 0 Yes Structure/activityrelationships
• PhysicaVChemical Properties • Testdata notinthe possession Or control ofthe submitter

•A physical and chemical properties worksheetis located on the last page of Ibis form. TYPE OF NOTICE (CheckOnly One)
PMN (Premanufacture Notice) INTERMEDIATE PMN (submitted in sequencewith final product PMN) 

# o SNUN (Significant New Use Notice) 

# o TMEA (Test Marketing Exemption Application) 

# o LVE (Low Volume Exemption) • CFR723.50 (c)(l) 

# o LOREX (Low ReleaseILow Exposure Exemption)'723.50(c)(2) LVE Modification Lore" Modification 

# o o

IS THISA CONSOLIDATEDPMN? 

## [8J Yes

II- ofchemicals 

### 3 (Prenotice CommunicationII- required, enterII- onpage3) EPA FORM7710-25 (Rev. 5-95) Replaces previous editions ofEPA Form 7710-25Public reporting burden for this collection ofinformation is estimated to average 110 hours perresponse, including time for reviewing instructions, searching existing data sources, gathering and maintaining the data needed, and completing and reviewing the collection ofinformation. Send comments regarding the burden estimate or any otheraspect orthis collection ofinformation, including suggestions for reducing this burden, to Chief, Information Policy Branch, PM-223, U.S. Environmental Protection Agency, 401 M. St., S.W., Washington, D.C. 20460; and to the Office of Management and Budget, Paperwork Reduction Act (2070-0012), Washington, D.C. 20503. 

## CERTIFICATON
I certifY that to the best ofmy knowledge and belief: I. The company named in Part I, section A, subsection I a ofthis notice form intends to manufacture or import for a commercial purpose, otherthan in small quantities solely for research and development, the substance identified in Part I, Section B. 2. All information provided in this notice is complete and truthful as ofthe date ofsubmission. 3. I am submitting with this notice all test data in my possession or control and a description ofall other data known to orreasonably ascertainable by me as required by §720.50 ofthe Premanufacture Notification Rule.

Additional Certification Statements: Ifyou are SUbmitting a PMN, IntermediatePMN, Consolidated PMN, or SNUN, checkthe following userfee certification statement that applies: The Company named in Part I, Section A has remitted the fee of$2500 specified in 40 CFR700.45 (b), or The Company named in Part I, Section A has remitted the fee 0[$1000 for an Intermediate PMN (defined @40 CFR 700.43) in accordance with 40 CFR 700.45(b), or 

# D The Company named in Part I, Section A is a small business concern under 40 CFR 700.43 and has remitted a fee of$IOO in accordance with 40 CFR 700.45 (b). Ifyou are submitting a low volume exemption (LVE) application in accordance with 40 CFR 723.50 (c) (I) or a Low release and low exposure exemption (LoREX) application in accordance with 40 CFR723.50 (c) (2), checkthe following certification statements: 

# D D D D The manufacturer submitting this notice intends to manufacture or import the new chemical substance for commercial purposes, other than in small quantities solely for research and development, under the terms of40 CFR 723.50. The manufacturer is familiar with the terms ofthis section and will comply with those terms; and The new chemical substance for which the notice is submitted meets all applicable exemption conditions. Ifthis application is for an LVE in accordance with 40 CFR 723.50 (c)(I), the manufacturer intends to commence manufacture ofthe exempted substance for commercial purposes within 1year ofthe date ofthe expiration ofthe 30 day review period.

# .Ca~ The accuracy ofthe statements you make in this notice should reflect yourbest prediction ofthe anticipated chemical

substance described herein. Any knowing and willful misinterpretation is subject to criminal penalty pursuant t 1 01.

# ~&A Confidential Signatureand title ofAuthorized Official (Original SignatureRequired) Date
Signatureofagent
- (ifapplicable) Date

FORM EPA 7710-25 (Rev. 5-95) Page 2

## Part I -- GENERAL INFORMATION Section A

-- SUBMITTER IDENTIFICATION**~------------------------------------------------------------------------------------~** Confidential Mark (X) the "Confidential" box nextto any subsection you claim as confidential. lao Person Submitting Notice (in U.S.)

b. Agent (if applicable) Company

c. Ifyou are submitting this notice as partofajoint submission, mark (X)this box. Ioint Submitter (ifapplicable)

2. Technical Contact (in U.S.) Name

you or import for the chemical substance covered by this notice, enterthe notice number assigned by EPA. Mark (X) ifnone 

# D

Mark (X) ifnone

Mark (X) ifnone 

# •

6. Type ofNotice

-- Mark (X) l. 

# D Binding Option Mark (x) 2. 

# D Binding Option Mark (x) 3. Both
FORM EPA 7710·25 (Rev. 5-95) Pagel

## PartI

-- GENERAL INFORMATION

-- Continued You mustprovide a currently correctChemical Abstracts (CA) name ofthe substance 

### Section B - CHEMICAL IDENTITY INFORMATION based on the ninth Collective Index (9<:1) ofCA nomenclature rules and conventions. Complete either item 1 (Class 1 or 2 substances) or2 (Polymers) as appropriate. Complete all other items. Ifanother person will submit chemical identity information for you (for either item I or 2), mark (x) the box atthe right IdentifY the name, company, and address ofthat person in a continuation sheet. ... 

# 0 I. Class 1 or2 chemical substances (fordefinitions ofclass I and class 2 substances, see the Instructions Manual) 

### a Class ofsubstance

-- Mark (X) 1 

# I2$J Class I or 2 

# 0 Class 2 b. Chemical name (Currently correctChemical Abstracts (CA) Name that is consistentwith TSCA Inventory listings for similar substances. For Class I substances a CA Index Name mustbe provided. For Class 2 substances either a CA Index Name or CA Preferred Name must be provided, whichever is appropriate based onCA 9CI nomenclature rules and conventions).

c. Please identifY which method you used to develop or obtain the specified chemical identity information reported in this notice: (check One). 

### 1"':71 Method I (CAS Inventory Expert Service - a copy ofthe Identification

### ~ report obtained from the CAS Inventory Expert Service must be submitted as an attachmentto this notice) 

# o Method 2 (Other Source)

d. Molecularformula and CAS Registry Number (ifa number already exists for the substance)

CAS#

e. For a class 1 substance, provide a complete and correctchemical structural diagram. For a class 2 substance

- (I) Listthe immediate precursor substances with theirrespective CAS Registry Numbers. (2) Describe the nature ofthe reaction orprocess. (3) Indicate the

range ofcomposition and the typical composition (where appropriate). (4) Provide a correctrepresentative orpartial chemical structural diagram, as complete as can be known, ifone can be reasonable ascertained.



# o Mark (X) this box ifyou attach a continuation sheet.

## PartI

-- GENERAL INFORMATION

-- Continued You must provide a currendycorrect Chemical Abstracts (CA) name ofthesubstance 

### Section B

-- CHEMICAL IDENTITY INFORMATION based on the ninth Collective Index (9CI) ofCA nomenclature rules and conventions. Complete eitheritem 1 (Class 1 or2 substances) or2 (Polymers) as appropriate. Complete all other items. Ifanother person will submit chemical identity infonnation for you (for either item I or2), mark (x) the box at the right. Identii}' the name, company, and address ofthat person in a continuation sheet. • 

# 0 I. Class 1 or2 chemical substances (for definitions ofclass I and class 2 substances, see the Instructions Manual)
a. Class ofsubstance

- Mark (X) 1 

## [8j Class I or 2 

# 0 Class 2 b. Chemical name (Currently correct Chemical Abstracts (CA) Name that is consistentwith TSCA Inventory listings for similar substances. ForClass I substances a CA Index Name mustbe provided. For Class 2 substances either a CAIndex Name orCAPreferred Name must be provided, whichever is appropriate based on CA 9C1 nomenclature rules and conventions).

c. Please identii}' which method you used to develop or obtain the specified chemical identity infonnation reported in this notice: (check One). 

# D Method I (CAS Inventory Expert Service - a copy ofthe Identification Method 2 (Other Source) report obtained from the CAS InventoryExpert Service must be submitted as an attachmentto this notice) d. Molecular fonnula and CAS Registry Number (ifa number already exists for the substance)

CAS#

e. For a class 1 substance, provide a complete and correct chemical structural diagram. For a class2 substance

- (I) Listthe immediate precursor substances with their respective CAS Registry Numbers. (2) Describe the nature ofthe reaction or process. (3) Indicate the

range ofcomposition and the typical composition (where appropriate). (4) Provide a correct representative orpartial chemical structural diagram, as complete as can be known, ifone can be reasonable ascertained.



# D Mark (X) this box ifyou attach a continuation sheet.

## PartI - GENERAL INFORMATION

-- Continued You mustprovide a currently correctCbemical AbstracD (CA)name oftbe substance 

### Section B

-- CHEMICAL IDENTITY INFORMATION based onthe nintb Collective Index (9CI)ofCA nomenclaturerules and conventions. Complete either item 1 (Class 1or 2 substances) or2 (Polymers) as appropriate. Complete all other items. Ifanother person will submit chemical identity information for you (foreither item I or 2), mark (x) the box at the right. IdentitY the name, company, and address ofthatperson in acontinuation sheet. ---....... 

# 0 I. Class 1or 2chemical substances (for definitions ofclass I and class 2 substances, see the Instructions Manual) a. Class ofsubstance

-- Mark (X) I 

# I:8J Class I or 2 

# 0 Class 2 b. Chemical name (Currently correct Chemical Abstracts (CA) Name that is consistent with TSCA Inventory listings for similar substances. ForClass 1substances aCA Index Name must be provided. ForClass 2 substances either aCA Index Name orCA Preferred Name must be provided, whichever is appropriate based on CA 9CI nomenclature rules and conventions).

c. Please identitY which method you used to develop orobtain the specified chemical identity information reported in this notice: (check One). 

# D Method 1(CAS Inventory Expert Service - acopy ofthe Identification Method 2(Other Source) report obtained from the CAS Inventory Expert Service must be submitted as an attachment to this notice) d. Molecular formula and CAS Registry Number (ifanumber already exists for the substance)

CAS#

e. For a class 1substance, provide acomplete and correct chemical structural diagram. For aclass 2 substance

- (I) List the immediate precursor substances with their respective CAS Registry Numbers. (2) Describe the nature ofthe reaction or process. (3) Indicate the

range ofcomposition and the typical composition (where appropriate). (4) Provide acorrectrepresentative or partial chemical structural diagram, as complete as can be known, ifone can be reasonable ascertained.



# D Mark (X) this box ifyou attach a continuation sheet.

## PartI

-- GENERAL INFORMATION

-- Continued

# ~ Section B - CHEMICAL IDENTITY INFORMATION

-- Continued 2. Polymers (For a definition ofpolymer, see the InstructionsManual.)

# ;:~r~1 a. Indicate the number-average weight ofthe lowestmolecular weight composition ofthe polymeryou intend to manufacture.

Indicate maximum weight percentoflow molecular weight species (not including residual monomers, reactants, orsolvents) below 500 and below 1,000 absolute molecular weight ofthatcomposition. Describe the methods ofmeasurement or the basis foryourestimates: OPC 

## 0 Other 

## 0 : (Specity) i) lowest number average molecular weight: ii) maximum weight % below 500 molecular weight: iii) maximum weight % below 1000 molecular weight: 

## Page 5 not applicable 

# [] Mark (}() this box ifyou attach a continuation sheet. b. You must make separate confidentiality claims for monomer orotherreactant identity, composition information, and residual information. Mark (X) the ·Confidential" box nextto any item you claim as confidential. (I)

-- Provide the specific chemical name and CAS Registry Number (ifa number exists) ofeach monomer orother reactant used in the manufacture ofthe polymer. (2)

-- Mark (X) this column ifentry in column (I) is confidential. (3)

- Indicate the typical weight percentofeach monomerorotherreactant in the polymer. (4)

-- Mark (X) theidentitycolumn ifyou want a monomer orother reactantused at twoweight percentorless tobe listed aspartofthe polymer description on theTSCA Chemical Substance Inventory. (5)

-- Mark (X) this column ifentries in columns (3) and (4) are confidential. (6)

-- Indicate the maximum weight percent ofeach monomer orother reactantthat may be present as a residual in the polymer as manufactured for commercial purposes. (7) -. Mark (X) this column ifentry in column (6) is confidential. Monomerorotherreactant and CAS Registry Number Confi- Typical Identity Confi- Maximum Confidential composition Mark (X) dential residual dential (I) (2) (3) (4) (5) (6) (7) % % % % % % % % 

### o/j.

# " % %"

# "OAA. % % 

# ',.**~ALt** % 

## 0 Mark (X) this box ifyou attach a continuation sheet.

# '~A c. Please identify which method you used to develop or obtain the specified chemical identity information reported in this notice. (check one). V 

# o Method I (CAS Inventory Expert Service - a copy ofthe identification report 

# o Method 2 (other source) obtained from CAS Inventory Expert Service must be submitted as an ttothis notice) d. The currently correct Chemical Abstracts (CA) name for the polymerthat is consistent with TSCA Inventory listings for similar polymers.

e. Provide a correct representative orpartial chemical structure diagram, as complete as can be known, ifone can bereasonably ascertained.



## 0 Mark (X) this box ifyou attach a continuation sheet. FORM EPA 7710-25 (Rev. 5-95) PageS

## PartI

-- GENERAL INFORMATION

-- Continued 

# • Section B

-- CHEMICAL IDENTITY INFORMATION

- Continued 3. Impurities

<a)

­ Identify each impurity that may be reasonably anticipated to be present in the cbemical substance as manufactured forcommercial purposes. Provide the CAS Registry Number iCavaiiable. Ifthere are unidentified impurities, enter "unidentified." (b)

­ Estimate the maximum weight "I. ofeach impurity. Ifthere are unidentified impurities, estimate their total weight "Ia. Impurity and CAS Registry Number Contipercent dentia1 (a) (b) 

### % %

0/

0 

### %

0/0
0/0 

### % 

# 0 Mark (X) this box ifyou attach a continuation sheet. 4. Synonyms

­ Enter any chemical synonyms for the new chemical substance identified in subsection 1or 2.

# ;:~~:I



# 0 Mark (X) this box ifyou attach a continuation sheet. 5. Trade identification

­ List trade names for the new chemical substanceidentified in subsection 1 or 2.



# 0 Mark (X) this box ifyou attach a continuation sheet. 6. Generic name -­ 

### n you claim chemical identity as you must**provi~e** a generic chemical name for your that reveals the specific chemical identity ofthe new chemical substance tothe maximum extentpossible. Referto the TSCAChemical Substance Inventory, 1985 Edition, Appendix B for guidance on developing generic names. 

## Amine Diol

# CO~A 0 Mark (X) this box ifyou attach a continuation sheet. 

# AJt1t 

# r**-t~A** 7.**~.H"** uu""'"

­ Describe any 't' :resulting from the 'r .!g, use, ordisposal ofthe new chemical • 'v 'A<;: Registry Number ifavailable.

# ·'VI/)~ 

# .. Byproduct CAS Registry Number 

# .... -..1'1 (I) (2)

# r~1 None known



# 0 Mark (X) this box ifyou attach a continuation sheet. FORM EPA 7710-25 (Rev. 5-95) Page 6

## PartI

-- GENERAL INFORMATION

-- Continued

# ~ Section C

-- PRODUCTION, IMPORT, AND USE INFORMATION Mark (X) the "Confidential" box next to any item you claim as confidential. 1. Production volume

-- Estimate the maximum production volume during the first 12 months ofproduction. Also estimate the maximum production volume for any consecutive 12-month period during the first three years ofproduction. Estimates should be on 100% new chemical substance basis. For a Low Volume Exemption application. ijyou choose to haveyournotice reviewedata lower production volume than 10,000 kg/yr, specify the volume andnwrk (x) in the bindingbox. 

### If granted, youare boundto this volume. Maximum first 12-month production (kgfyr) Maximum 12-month production (kgfyr) Confi- Binding (100% new chemical substance basis) (100% new chemical substance basis) dential Option Mark (x) 

## 29,920 55,000 2. Use information

-- You must make separate confidentiality claims for the description ofthe category ofuse, the percentofproduction volume

devoted to each category, the formulation ofthe new substance, and otheruse information. Mark (X) the "Confidential" Box nextto any item you claim as confidential. 

### a. (I)

-- Describe each intended category ofuse ofthe new chemical substance by function and application.

(2)

-- Mark (X)this column ifentry in column (I)is confidential business information (CBI). (3)

- Indicate your willingness to have the information provided in column (I) binding. (4)

-- Estimate the percentoftotal production for the first three years devoted toeach category ofuse. (5)

-- Mark (X) this column ifentry in column (4) is confidential business information (CBI). (6)

- Estimate the percent ofthe new substance as formulated in mixtures, suspensions, emulsions, solutions, or gels as manufactured for commercia! purposes at sites under your control associated with each category ofuse. (7)

-- Mark (X) this column ifentry in column (6) is confidential business information (CBI). (8)

-- Indicate % ofproduct volume expected for the listed "use" sectors. Mark more than one box ifappropriate. Mark (X)to indicate yourwillingness to have the use type provided in (8)binding. {O\
__ M",1c {Y\ thi. ""I11mn if, in ""I11mn (I!\ i. (,

.....i .Co. • Ihll im'••. £rRIi Category ofuse (I) CBI Binding Produc- CBI %in CBI %ofsubstance expected peruse CBI (by function and application i.e. a dispersive dye for Option tion% Form­ (8) finishing polyester fibers) Mark (x ulation

# Site-~m- Binding limited sumer trl rcia! Option (I) (2) (3) (4) (5) (6) (7) (9) 

### 100% % 

### 100% 

## , , .' '

../; I/U 'j' , .! '/**~.** 

### j t .' I , 

### \i 

## 1 '.,. '

.. '**~.\'** 

## ",**~:. ~**  i 

## 'I , . (.}i t I \, 

## I ; '",' 

# . % %**~ ~**  iii i;. , ; 

### I % %
i % % % % % % % % 

### "'Ifyou have identified a "consumer" use, please provide on a continuation sheet a detailed description ofthe use(s) ofthischemical substance in consumerproducts. In addition include estimates ofthe concentration ofthe new chemical substance as expected in consumer products and describe the chemical reactions by which this substance loses its identity in the consumer product.



# 0 Mark (X) this box ifyou attach 

### acontinuation sheet. b. Generic Ifyou claim any category ofuse description in subsection 2a as confidential, enter a generic description oftbat

use category. Read tbe Instructions Manual for examples ofgeneric use descriptions. description 

### Chemical intermediate with destructive use 

# 0 Mark (X)this 

### box ifyou attach a continuation sheet. J. Hazard Information • Include in the notice acopy ofreasonable facsimile ofany hazard warning statement, label, material safety data sheet, Binding

orother information which will beprovided to any person who is reasonably likely to be exposed to this substance regarding protective Option equipmentorpl1lctices for the safe handling, transport, use, ordisposal ofthe new substance. List in part IIIhazard information you include. Mark (x) 

# J:8l Mark (X)this box tfyou attach hazard information. 

### See Hazard Warning, Page 13 FORM EPA 7710-25 (Rev. 5-95) Page 7

## PartII

-- HUMAN EXPOSUREAND ENVIRONMENTAL RELEASE Section A

-- INDUSTRIAL SITES CONTROLLED BY THE SUBMITTER Mark (X) the "Confidential" box nextto any item you claim a.c:onfidential

ofthe site at which the will occur.

Mark (X) this box ifyou attach a continuation sheet. 

# o Processing 

# o Use

Hourslbatch Batches/year substance) 

## 24 

## 12 ,V'."'IU"UlU kg/day (100% newchemical Hours/day Days/year substance) Mark (X) to indicate your willingness to have your process description binding. (\) Diagram the majorunitoperation steps and chemical coversions. Include interim storage and transport containers (specify-e.g. 5 gallon pails, 55 gallon drum, rail car, tanktruck, etc.). (2) Provide the identity, the approximate weight (by kg/day orkglbatch, on a 100% new chemical substance basis), and entry pointofall starting materials and feedstocks (including reactants, solvents, and catalysts, etc.), and ofall produets, recycle streams, and wastes. Include cleaning chemicals (note frequency ifnot used daily or perbatch.). (3) Identify by number the points ofrelease, including small orintermittant releases, to the environment ofthe new chemical substance.



## Please see Page 8A1



# o Mark (X) this box ifyou attach a continuation sheet. Confidential

## Continuation Sheetfor PartII. Section A. Item lid

- Process Description

Page 8AI

## Continyation Sheetfor Part II. Section A. Item 1(d) Process Description

Page 8A2

## Continuation Sheetfor Part II. Section A, Item 1(d) Process Description

Page SA3

### Section A

-- INDUSTRIAL SITES CONTROLLED BY THE SUBMITTER you

Ifthe same operation will occur at more than one site, enter the number ofsites. Identify the additional sites on a continuation sheet, and ifany ofthe sites have significantly different production rates or operations, include all the information requested in this section for those sites as attachments. Mark (X) this box ifyou attach acontinuation sheet. 

# 00 Processing

Hourslbatch 1. Batch substance) 

## 8 I"""Jum"ulIkg/day (100% new chemical Hours/day 2. Continuous substance) 

# o Use Batches/year Days/year Mark (X) to indicate your willingness to have your process description binding. 

## 8

(I) Diagram the major unit operation steps and chemical coversions. Include interim storage and transport containers (specify-e.g. 5gallon pails, 55 gallon drum, rail car, tank truck, etc.). (2) Provide the identity, the approximate weight (by kg/day orkglbatch, on a 100%new chemical substance basis), and entry pointofall starting materials and feedstocks (including reactants, solvents, and catalysts, etc.), and ofall products, recycle streams, and wastes. Include cleaning chemicals (note frequency ifnot used daily or per batch.). (3) Identify by numberthe points ofrelease, including small or intermittant releases, to the environment ofthe new chemical substance.



# o Mark (X) this box ifyou attach a continuation sheet. 

## PartII

-- HUMAN EXPOSURE AND ENVIRONMENTAL RELEASE Mark (X) the "Confidential" box next to anyitem you claim a,confidential each type ofmanufacture, or use new Importers do not have to complete this section for operations outside the U.S.; however, you may still have reporting requirements ifthere are further industrial processing or use operations after import. You must describe these operations. See instructions manual. Confiofthe site at which the will occur. dential

(number and street)

## PartII

-- HUMAN EXPOSURE AND ENVIRONMENTAL RELEASE Section A

-- INDUSTRIAL SITES CONTROLLED BY THE SUBMITTER Mark(X) Ihe "Confidential" OOX next to any item you claim asconfidential type ng, or use new you Importers do not have to complete this section for operations outside the U.S.; however, you may still have reporting requirements ifthere are further industrial processing or use operations afterimport. You must describe these operations. See instructions manual. ofthe site at which the will occur,



# [!] Processing
kg/batch (100% new chemical Hourslbatch

2. Continuous 

## 9039 substance) jMlllXilTlWll kg/day (100% new chemical substance) Hours/day 

# D Use
Batches/year 

## 8 Days/year
Mark (X) to indicate yourwillingness to have your process description binding. 

## 6

(1) Diagramthe major unit operation steps and chemical coversions. Include interim storage and transport containers (specifY-e.g. 5 gallon pails, 55 gallon drum, rail car, tank truck, etc.). (2) Provide the identity, the approximate weight (by kg/day orkglbatch, on a 100%new chemical substance basis), and entry point ofall starting materials and feedstocks (including reactants, solvents, and catalysts, etc.), and ofall products, recycle streams, and wastes. Include cleaning chemicals (note frequency ifnot used daily orper batch.). (3) IdentifY by numberthe points ofrelease, including small or intermittant releases, to the environment ofthe new chemical substance.



# D Mark (X) this box ifyou attach a continuation sheet. Coofi· dentiaI

# ofsites number ofsites.

Mark (X) this box ifyou attach a continuation sheet.

## PartII

-- HUMAN EXPOSURE AND ENVIRONMENTAL RELEASE

-- Continued

# ~ Section A - INDUSTRIAL SITES CONTROLLED BY THE SUBMITTER

­ Continued**~.** Occupational Exposure

-- You must make separate confidentiality claims for the description ofworker activity, physical form ofthe new chemical substance, number ofworkers exposed, and duration ofactivity. Mark (X) the "Confidential" box next to any item you claim as confidential. (I)
..Describe the activities (i.e. bag dumping, tote filling, unloading drums, sampling, cleaning, etc.) in which workers may be exposed 

### to the substance. (2)
..Mark (X) this column ifentry in column (I) is confidential business information (CBI). (3)
.. Describe any protective equipment and engineering controls used to protect workers. (4) and (6) -·Indicate your willingness to have the information provided in column (3) or (5) binding. (5)
..Indicate the physical formes) ofthe new chemical substance (e.g. solid: crystal, granule, powder, ordust) and % new chemical substance (ifpart of a mixture) atthe time ofexposure. (7)

-- Mark (X) this column ifentry in column (5) is confidential business information (CBI). (8)
..Estimate the maximum number ofworkers involved in each activity for all sites combined. (9) •• Mark (X) this column ifentry in column (8) is confidential business information (CBl). (10) and (II) _. Estimate the maximum duration ofthe activity for any worker in hours per day and days peryear. (121

..Mark (X)**thi~** colnmn ifentrie in llnmns (J 0) and (J 11 are**,~.** • 11",';n

.... • FrRH Worker activity CBI Protective Equipment! Binding Physical fonn(s) Binding CBI #of CBI 

### MlIXiwlIW dw:a.ti2o. CBl (Le., bag dumping, filling drums) Engineering Controls Option (e.g.solid:powder) Option Workers Mark (x) and % new sub. Mark (x) Exposed Hrslday Dayslyr (I) (2) (3) (4) (5) (6) (7) (8) (9) (10) (11) (12) Liquid Remove samples for quality control Please see Page90 80-99% 3 0.5 12 Liquid Process samples in lab Please see Page90 80-99% 3 1.0 12 Liquid Filtration and filling Please see Page90 95-99 8 /. 3 1.0 12 Liquid Cleaning equipment Please see Page90 80-99% 3 0.5 12 Cbarging IntermediateStagePMN Liquid substance to reactor Please see Page90 95-99% 2 1.0 12 

# D Mark (X) this box ifyou attach a continuation sheet. 3. Environmental Release and Disposal

-- You must make separate confidentiality claims for the release number and the amount ofthe new chemical

substance released and other release and disposal information. Mark (X) the "Confidential" box next to each item you claims as confidential. (I)

-- Enter the number ofeach release point identified in the process description, part II, section A, subsection Id(3). (2) •• Estimate the amount ofthe new substance released (a) directly to the environment or(b) into control technology (in kg/day orkglbatch). (3)

-- Mark (X) this column ifentries in columns (I) and (2) are confidential business information (CBI). (4) --IdentifY the media ofrelease i.e. stack air, fugitive air (optional-see Instruction Manual), surface water, on-site oroffsite land or incineration, POTW, orother (please specifY) to which the new substance will be released from that release point. (5)

­ a. Describe control technology, ifany, and control efficiency that will be used to limitthe release ofthe new substance 

### to the environment. For releases disposed ofon land, characterize the disposal method and state whether it is approved for disposal ofRCRA hazardous waste. On a continuation sheet, for each site describe any additional disposal methods that will be used and whether the waste is subject to secondary ortertiary on-site treatment. b. Estimate the amountreleased to the environment after control technology (in kg/day). (6)

- Mark (X) this column ifentries in columns (4) and (5) are confidential business information (CBI). (7)

-- IdentifY the destinations(s) ofreleases to water. Please supplyNPDES (National Pollutant Discharge Elimination System) numbers for direct dischargers orNPDES numbers ofthe POTW (publicly Owned TreatmentWorks). Mark (X) ifthe POTW name ofNPDES # is confidential h". ,np« • '. {rRH Release Amountofnew substance CBI Mediaof Control technology and efficiency (you may wish to optionally attach efficiency data) CBI Number released release Binding

(I) (2a) (2b) e.g. stack air Mark (3) (4) (Sa) (x) (5b) (6) Off-sile t 15 .11. Please see Pape9E Nan
.. known Off-sile 2 15 "I. PI
..as.. "
.... Pap
.. 9E NoneknoWD Off-sile 3 IS kl!/batch Please see Pal'e 9E Nan
.. known Off-sile 

# " 45 k!!lbatcb Land Pleas!' see Pal'e 9E Non
.. known
7) Mark (X) the DPOTW provide name(s) below: '::..BI DNavigable 

# o Other

- SpecifY 

### provide NPDES

### # ",BI destination(s) of 

## - waterway releases to water.



# D Mark (X) this box ifyou attach a continuation sheet. FORM EPA 7710-25 (Rev. 5-95) Page9A

## PartII

-- HUMAN EXPOSURE AND ENVIRONMENTAL RELEASE

-- Continued

# ~ Section A - INDUSTRIAL SITES CONTROLLED BY THE SUBMITTER

­ Continued**~.** Occupational Exposure

-- You must make separate confidentiality claims for the description ofworker activity, physical form ofthe new chemical substance, number ofworkers exposed, and duration ofactivity. Mark (X) the "Confidential" box next to any item you claim as confidential. (I)

-- Describe the activities (i.e. bag dumping, tote fill ing, unloading drums, sampling, cleaning, etc.) in which workers may be exposed to the substance. (2)

- Mark (X) this column ifentry in column (1) is confidential business information (CBI). (3)

-- Describe any protective equipment and engineering controls used to protect workers, (4) and (6) -Indicateyour willingness to have the information provided in column (3) or (5) binding, (5) --Indicate the physical formes) ofthe new chemical substance (e,g. solid: crystal, granule, powder, or dust) and % new chemical substance (ifpart of a mixture) at the time ofexposure. (7)

-- Mark (X) this column ifentry in column (5) is confidential business information (CBI). (8)

-- Estimate the maximum number ofworkers involved in each activity for all sites combined. (9)

-- Marie (X) this column ifentry in column (8) is confidential business information (CBI), (10) and (11)

-- Estimate the maximum duration ofthe activity for any worker in hours perday and days per year. (12)

-- Mark (X)**thi~** column ifentrie :in c'1lumns (10'1 and (11) are . hu**~iness** .. <'. (eRn. Worker activity CBI Protective Equipment! Binding Physical fonn(s) Binding CBI # of CBI MllXiWl.!W 

### .d!.u:lWml CBI (I.e" bag dumping, filling drums) Engineering Controls Option (e,g,solid:powder) Option Worleers Mark (x) and % new sub. Mark (x) Exposed Hrs/day Days/yr (1) (2) (3) (4) (5) (6) (7) (8) (9) (10) (II) {I 2) Liquid Charging new substance to reactor Please see Page 90 95-99% 2 0.5 8

Processing samples ror quality Liquid control Please see Page 90 6-10% 4 0.5 8 Liquid Processing samples in lab Please see Page 90 6-10% 6 0.5 8 Liquid Filtration and filling Please see Page9D 6-100/0 2 1.0 8 Liquid Cleaningequipment Please see Page9D 6-10% 2 0.5 8 

# D Marie (X) this box ifyou attach a continuation sheet. 3. Environmental Release and Disposal

-- You mustmake separate confidentiality claims for the release number and the amount ofthe new chemical

substance released and otherrelease and disposal information. Mark (X) the ·Confidential" box nextto each item you claims as confidential. (I)

-- Enter the number ofeach release point identified in the process description, part II, section A, subsection Id(3). (2)

- Estimate the amount ofthe new substance released (a) directly to the environment or (b) into control technology (in leg/day orleglbatch). (3)

- Marie (X) this column ifentries in columns (1) and (2) are confidential business information (CBI). (4)

-- Identity the mediaofrelease i.e. stacie air, fugitive air (optional-see Instruction Manual), surface water, on-site oroffsite land or incineration, POTW, orother (please specity) to which the new substance will be released from thatrelease point. (5)

­ a. Describe control technology, ifany, and control efficiency that will be used to limit the release ofthe new substance to the environment. For releases disposed ofon land, characterize the disposal method and state whether it is approved for disposal ofRCRAhazardous waste. On a continuation sheet, for each site describe any additional disposal methods that will be used and whetherthe waste is subjectto secondary ortertiary on-site treatment. b. Estimate the amount released to the environment after control technology (in kg/day). (6)

- Marie (X) this column ifentries in columns (4) and (5) are confidential business information (CBI). (7)

- Identitythe destinations(s) ofreleases to water. Please supplyNPDES (National PollutantDischarge Elimination System) numbers for direct dischargers orNPDES numbers ofthe POTW (Publicly OwnedTreatment Worles). Marie (X) ifthe POTW name ofNPDES# is confidential (rRf) Release Amount ofnew substance CBI Mediaof Control technology and efficiency (you may wishto optionally attach efficiency data) CBI Number released release Binding

(I) (2a) (2b) e.g. stack air Mark (3) (4) (Sa) (x) (5b) (6) (1) 5.7 kg/batch 1 (2\ 12.7 kl!lbatch Please see PailI' 9F NODI' known (1) 0.8 kg/batch 2 (2\ 1.8 k!!lbatch Please see Palle9F None known (1) 1.6 kglbatch Off-site Filter residue and spent filters are incinerated lind IIny IIsh 2 

### m 3.6 k!!Ibatch Land is I"nitfillpd in RCRA­ I I"nitfill. NODI' known

7) Mark (X) the 

# o POTW provide Ilame(s) below:

### ~ 

# oNavigable LJOther

- Specity 

### provide NPDES #**~BI** destination(s) of waterway eleases to water.



# [ 

# ] Marie (X) this box ifyou attach a continuation sheet. FORM EPA 7710-25 (Rev. 5-95) Pages 98 and 9C

## Continuation Sheet for part

# II. Section 

# As Item 

# 2 Protective Eqyipment/Engineering Controls
All work takes place in well ventilated areas, and all associates are provided with and trained in the proper use of personal protective equipment such as goggles, gloves, protective clothing, and respirators. Our company utilizes a hazard rating system to individually assign proper and safe handling requirements to all chemical substances. This system assigns the personal protective equipment which must be worn when working with a chemical substance, and workers are required

## to wear this equipment. The intermediate stage PMN substances (I) and (II) are charged to clean reactors for manufacture of the final product. This procedure involves connection of hoses to drums to allow the substance to be pumped. The total time to charge this substance is estimated at three hours per reactor. However, the duration ofactual exposure is estimated at one hour per each reactor, based on the fact that most ofthe charge time involves pumping the substance through a closed system into the reactors. The filtration and filling of the PMN substance as well as the cleaning of processing equipment occurs in a closed system. Thus, the likelihood of exposure to the PMN substance in these activities is incidental.

Page 9D

## Continuation Sheetfor PartII. Section A, Item 3 ControlTechnology for Environmental Release

Page 9E

## Continuation Sheetfor PartII, Section A, Item 3 ControlTechnology for Enyironmental Release andDisposal

Page 9F

## PartII

-- HUMAN EXPOSUREAND ENVIRONMENTAL RELEASE

-- Continued

# ~ Section B ­ INDUSTRIAL SITES CONTROLLED BY OTHERS Complete section Bfor typical processing or use operations involving the new chemical substance at sites you do not control. Importers do not have to complete this section for operations outside the U.S.; however you must report any processing or use activities after import. See the Instructions Manual. Complete a separate section B for each type of processing. oruse operation involving the new chemicalsubstance. Ifthe same operation is performed at more than one site describe the typical operation common to these sites. Identify additional sites on a continuation sheet. 

### 1. Operation Description

- To claim information in this section as confidential, circle or bracketthe specific information that you claim as confidential. (I)

­ Diagram the major unit operation steps and chemical conversions, including interim storage and transport containers (specify-5 gallon pails, 55 gallon drums, rail cars, tanktrucks, etc). On the diagram, identify by letter and briefly describe each worker activity. (2)

-- Provide the identity, the approximate weight (by kg/day or kglbatch), 100% new chemical substance basis), and entry point ofall feedstocks (including reactants, solvents, and catalysts, etc) and ofall products, recycle streams, and wastes. Include cleaning chemicals (note frequency ifnot used daily or per batch). (3)

-- Identify by number the points ofrelease, including small or intermittentreleases, to the environmentofthe new chemical substance. (4) Please enterthe 

### #ofsites (remember to identify the locations ofthese sites on a continuation sheet): 

### 0 

### # ofsites The subject ofthis PMN is a chemical intennediate to be used by ourcompany only. It

### will 

### not be distributed to any

sites controlled by others.



# 0 Mark (X) this box ifyou attach a continuation sheet. 2. WorkerExposurelEnvironmental Release (1)

- From the diagram above, provide the letter for each worker activity. Complete 2-8 for each worker activity described. (2)

-- Estimate the number ofworkers exposed for all sites combined. (4)

-- Estimate the typical duration ofexposure perworker in (a) hours per day and (b) days per year. (6)

-- Describe physical form ofexposure and %new chemical substance (ifin mixture), and any protective equipment and engineering controls, ifany, used to protect workers. (7)

-- Estimate the percent ofthe new substance as formulated when packaged orused as a final product. (9)

- From the process diagram above, enter the number ofeach release point. Complete 9-13 for each release pointidentified. (10)- Estimate the amount ofthe new substance released (a) directly to the environmentor (b) into control technology to the environment (in kg/day orkglbatch). (12)

-- Describe mediaofrelease (stack air, fugitive air (optional-see Instructions Manual), surface water, on-site oroff-site land orincineration, POTW, or other(specify» and control technology, ifany, that will be used to limitthe release ofthe new substance to the environment. i (14)

- Identify byproducts which may result from the operation. i (3), (5), (8), (II), (13) and (15)

- Mark (X) this column ifany ofthe proceeding entries are confidential business information (CBI). Letter 

### # of CBI Duration CBI Protective Equip.! %in CBl Release Amount of CBI Control CBI

of Workers of Engineering Controls! Form- Number New Technology Act- Exposed Exposure Physical Form and % ulation Substance ivity new substance Released (I) (2) (3) (4a) (4b) (5) (6) (7) (8) (9) (lOa) (lOb) (II) (12) (13)

I

(14) Byproducts:



# D Mark (X) this box ifyou attach acontinuation sheet. FORM EPA 7710-25 (Rev. 5-95) Page 10

## OPTIONAL POLLUTION PREVENTION INFORMATION To claim information in this section as confidential circle or bracketthe specific information that you claim as confidential. 

## Inthis section you may provide information not reported elsewhere in this form regarding your efforts to reduce orminimizepotential risks associated with activities surrounding manufacturing, processing, use and disposal ofthe PMN substance. Please include new information pertinentto pollutionprevention, including source reduction, recycling activities and safer processes orproducts available due to the newchemical substance. Source reduction includes the reduction in the amount ortoxicity ofchemical wastes by technological modification, process and procedure modification, product reformulation, raw materials substitution, and/or inventory control. Recycling refers to the reclamation ofuseful chemical components from wastes that would otherwise betreated or released as air emissions orwater discharges, orland disposal. Descriptions ofpollutionprevention, source reduction and recycling should emphasize potential risk reduction subsequent to compliance with existing regulatory requirements and can be eitherquantitative or qualitative. The EPA is interested in this informationto assess overall netreductions intoxicity orenvironmental releases and exposures, not the shifting ofrisks to otherenvironmental media ornon-environmental areas (e.g., occupational orconsumerexposure). In additional, information onthe relative cost or performance characteristics ofthe PMN substance to potential alternatives may be provided. 

## All information provided in this section will be taken into consideration during the review ofthis substance. See Instructions Manual and Pollution Prevention Guidance manual for guidance and examples. Describe the expected net benefits, such as 

### (1) an overall reduction in risk to human health orthe environment; (2) a reduction in the volume manufactured; (3) a reduction in the generation ofwaste materials through recycling, source reduction or other means; (4) a reduction in potential toxicity or human exposure and/or environmental release; (5) an increase in product performance, a decrease in the cost ofproduction and/or improved operation efficiency ofthe new chemical substance in comparison to existing chemical substances used in similar applications; or (6) the extentto which the new chemical substance may be a substitute for an existing substance that poses a greater overall risk to human health orthe environment. 

## See Continuation Sheet, Page lIB, attached



# 0 Mark (X) this box ifyou attach a continuation sheet. FORM EPA 7710-25 (Rev. 5-95) Page 11

## Continuation Sbeetfor OptionalPollution Prevention Information,Page llA



## Page lIB

## Part III - LIST OF ATTACHMENTS
Attachcontinuation sheetsfor sections ofthe form and test data andotherdata (includingphysical!chemicalpropertiesand structure/activity information), andoptionalinformation after this page. Clearly identify theattachmentand the section of the form to whichitrelates, ifappropriate. Numberconsecutively the pagesof the attachments. In the columnbelow, enter the inclusivepage numbers ofeachattachment. Mark (X) the "Confidential"boxnext to any attachmentnameyou claimasconfidential. Read the Instructions Manual for guidance onhow to claimany informationinanattachmentasconfidential. You mustinclude with the sanitizedcopy of the notice form a sanitizedversion ofany attachmentinwhichyoudaiminformation as confidential. Attachmentname Attachment pagenumber(s) Confidential 

## lHazard Warning, PartI, Section c/3 13 PhysicalfChemical Properties 14 IntermediateStage (I) GC 15 Intermediate Stage (I) IR Spectrum 16 IntermediateStage (II) GPC 17 IntermediateStage (II) IR Spectrum 18 Final ProductGPC 19 [Final ProductIR Spectrum 20 DeterminationofAmine EquivalentWeightTestMethod 21-23 DeterminationofHydroxylValue TestMethod 24 Semi-Micro DeterminationofBasicity TestMethod 25-26 !DeterminationofWaterContentTest Method 27 -36



# 0 Mark(X) this box ifyou attach a continuation sheet. Enter the attachmentname andnumber. FORMEPA 7710-25 (Rev. 1-91) Page 12

## HAZARD WARNING

Page 13

# PHYSICAL/CHEMICAL PROPERTIES

Page 14

## INTERMEDIATE STAGE (I)

## GC

Page 15

## INTERMEDIATE STAGE (I) 

## IR SPECTRUM

Page 16

## INTERMEDIATE STAGE (II) GPC

Page 17

## INTERMEDIATE STAGE (II) IR SPECTRUM

Page 18

## FINAL PRODUCT OPC

Page 19

# EINAL PRODUCT IR SPECTRUM

Page 20

# DETERMINATION OF AMIJojE EQUIVALENT><WEIGHT



# CAUTION: Personnel using this test method should be familiar with the safety and handling precautions both for the material to be tested and the reagents used in the testing procedure.
1. Purpose and Application This method is used to determine the amine equivalent weight of acrylic, polyester, epoxy systems, po1yamides and other amine modified resins soluab1e in acetic acid. The purity of amines can also be tested by this procedure. 2. Concept and Definition The amine equivalent of a sample is that weight in grams which contains 1 equivalent of amine nitrogen. The amine equivalent weight is determined by potentiometric titration of the sample with O.lN perchloric acid using glacial acetic acid as the solvent. 

# ( 3. Sampling Sampling shall be done in accordance with STM 55/77. The sample shall be prepared for testing in accordance with 555/77
. 4. Number of Determinations The test shall be run in duplicate. 5. Apparatus Beakers, 150 ml with watch glass Graduated cylinder, 100 ml Balance, accurate to + 

# 0.1 mg Potentiograph, equipped with glass combination electrode Magnetic stir bars, teflon coated 6. Reagents Glacial acetic acid, reagent grade Perchloric acid, O.lN in glacial acetic acid, standardized 7. 

# Procedure The sample weight is determined from the theoretical amine equivalent weight. In general 0.1 grams of sample is required for each 100 gram equivalent weight (Note A).
Page 21 FO RM 3961 5·77

# c ;**~TM** 

# #358/81 Page 2 Weigh the appropriate size sample into a 150 ml beaker. Add a magnetic stir bar and 70 ml of glacial acetic acid and cover with a watch glass. Stir the sample until completely solubilized. Titrate the sample potentiometrically with O.lN perchloric acid until the typical S-shaped titration curve is obtained. Determine the volume of titrant consumed from this curve. Ablank must be run on 70 ml of the glacial acetic acid. 8. 

# Calculations Amine equivalent weight SWX1000 Am. Eq. Wt. = -------­ 

# (vs-vb)x n Percent amine nitrogen (Vs-Vb) x Nx 

# 14 x 100 %

# Am. N2 

# =---------------------­ SW X1000 Base Number(Vs-Vb) X NX 

# 56.1 Base No. 

# =-----------------­ SW % 

# Specific Amine
=

___ 

## (v -v



# _______________ ) 

# X N X F X100 %

# Amine 

# s__b
_ 

# SW X 

# 1000 Meg of Base(vs-vb) X N Meg base 

# =----------­ SW Where SW = 

# sample weight in grams Vs 

# =ml of perchloric acid required to neutralize the sample Vb = 

# ml of perchloric required to neutralize the solvent blank N= 

# Normality of the perchloric acid F = 

# Equivalent weight of the amine 9. Precision This repeatability and reproducibility of this method ;s now being established. It will be issued upon evaluation. 10. Report of Analysis The result shall be reported as the average of duplicate determinations.

Page 22

# STM #358/81 'Page 3**~** 

# 11. References 1. Sigga, Sidney Quantitative Organic Analysis Via Functional Groups. John Wiley and Sons, New York, 

# N. Y. 1979. 2. Fritz, J. Anal. Chern. 22, 1028-1029, 1950. 12. Notes A. For samples of pure amines or samples with low equivalent weights (<200) it is recommended that the required sample weight be multiplied by 10 and this weight added to a 100 m1 volumetric flask containing 50 ml of glacial acetic acid. Swirl the flask to solubilize the sample and make to volume with glacial acetic acid. Use a 10 ml aliquot of this solution for titration. 

# B. For pure amines or volatile samples the use of a sealed weighing bottle is recommended. C. Samples which are insoluble in glacial acetic acid can be tested following STM 474/80. 

# c D. The use of an indicator is not recommended but samples may be tested using methyl violet indicator (0.5% wt/vo1 in glacial acetic acid). Add 6 

# drops of indicator to the sample container and titrate with O.lM perch10ric acid from 25 ml buret graduated to 0.1 ml. Acolor change from blue-violet to bright green is typical for methyl violet in glacial acetic acid. 13. Author ani**D~tr** 

# August 6, 

# 1981



# (

Page 23

### ·DEl'EfHlNA.TION OF HYDroXYL 

# VAwE.
CCl-1CEFT AND 

### DEFrnrrION 

## the hydroxyl value and the corresf,X:)nding sanple weight. The hydroxyl value of a· sample, milligrams of p:>tassium hydroxide TABLE I 

## equivalent 00 

## the hydroxyl cx:mtent of 1 gram of sanple, is determined by 

## The::>retical 'Weight acid catalyzed acetylation. The OR Value acetylatiilg reagent is·a mixture of acetic anhydride and dichloroethane using. 50 3.0 paraOOluene sulfonic acid as 

## the 

## catalyst. 100 2.0 200 

## 1.0 SAFElY 

## 300 0.75 400 0.53 All 

## chanicals e:nployedin this 

## methcd 500 0.42 are OOxic and/or corrosive. Adequate 

## 600 0.35 eye protection and gloves ImlSt be 

## worn 700 0.30 \<1hi1e handling these chemicals. All work 800 0.20 should be perfonred in a furre 

## hocrl. 800 0.15 NUHBER OF 

## DEI'ERMINATICNS Weigh·'. the sample, 00 

## the nearest 1 

## n:g. inOO a clean 250 ml beaker. 

## The hydroxyl value shall be run 

## in Mel 

## a rragnetic stirring 

## tar and 

## 10 duplicate. ml 

## of dichloroethane 00 

## the beaker. Cover the beaker and 

## stir 

## until the APPARA'IUS 

## sample is completely in solution. The solution may be wanne:l 00 

## aid balance, acx::urate to 1 reg. 

## in solubilizing the sample. 

## After magnetic stirrer cooling, pipet 10 ml 

## of the**acety~** 

## magnetic stirring bars 

## lating reagent into the beaker and 

## 150 ml beakers

. 

## continue to stir the sample for 30 10 

## airl 50 ml 

## graduated cylin:1ers minutes. After 

## 30 minutes add 

## 40 ml 

## 10 ml 

## pipet of the hydrolyzing solution and 

## stir p:>tentiograph or endp:>int titrator an additional 10 minutes. After 

## hydrolysis, add 30 ml 

## of the solvent mixture and 

## titrate the sample with 

# o.5N rrethanolic p:>tassium hydroxide Dichloroethane on a p:>tentiograph or endpoint titra**Ace~lating** 

## Reagent...;. 40 mls. tor. Duplicate blanks muSt be rtll1 

## Uy**acet~c** 

## anhydride and the al:ove procedure omitting only 13.1 grams paratoluene sulfonic acid the 

## sanple. dissolved: in 400 rnls. dichloroethane.**~lYZing** 

## solution - A mixture 9f CAI.ClJI.,.AT

### IONS



# OOmls. di.Jrethyl fo:t:mamide,. 200 mls. pyridine and 200 mls. distilled water. 

## The hydroxyl value is calculated by 

## Solvent Mixture

- 20/80 

# {v/V1 propylene 

# the following equation: glycol/tetrahydrofuran. OH Value = 

## (Vb

- Vs) X N X

## ~.l Titrant

- 0.5000 N rrethanolic p:>tassium 

# sw hydroxide, standardized. Vb = 

## volurre cons\.ll.TV2Cl by 

## blank, rnl Vs 

# = volume consumed by 

## sample, ml PIO:EIXJRE 

## N = 

## normality of the Potassium Hydroxide equiv 

# 11 The sample weight to be used 

## is S = 

## sample weight in gms. det.exrnlned by 

## the theoretical hydroxyl value. Table I 

## lists 

# Page 24

# - '--'­ 

### STANDARD TESTING 

## SEMI-MICRO DETERMINATION OF BASICITY OF COATINGS AND RESINS BY POTENTIOMETRIC TITRATION METHOD 

## S'lM 11470B/8C CAUTION: Personnel using this test method should be familiar with the safety and handling precautions both for the material being tested and equipment and the reagents used in the testing method. 1. PURPOSE AND APPLICATION 7. 

## RFAGENTS This method covers the semi-micro deter­ 20/80 

## V/V propylene glyco1/tetramination ofbasicity in most solvent base hydrofuran and water base coatings and resins. The a.lOOON Aqueous HCL
. main advantage is the reduced size of titration**vo~ume,** 

## which reduces waste generation and solvent consumption. 8. PROCEDURE 2. 

## DEFINITION Into a 50 

## m1 beaker, weigh and record (Sw) to the nearest 1 mg, sufficient**Bas~** 

## Value

- the number of milligrams sample for a 2.5 m1 titration. (See of base as KOH contained in each gram Table I for approximate weights) of sample. !1eq. of Base

- the number of milli­ TABLE I equivalents of bydrochloric acid re­ quired to neutralize 1 

## gram of sample. Theoretical Theoretical Base Value Meq. S. Weight(g SAFETY 3.0 0.05 3.00g Most chemicals employed in this test 5.6 0.10 2.5 are toxic. Adequate eye protection and 9.0 0.15 1.67 gloves must be worn while handling these 11.2 0.20 1.25 materials. All work should be performed 17 .0 0.30 0.83 in a fume hood. 22.0 0.40 0.63 4. SA.'1PLING Add 25 

## m1 of the solvent mixture, place a stirring bar in the beaker and stir Sampling shall be done in accordance until the sample is in solution. In with STM SS/77. The sample shall be difficultcases, heat gently to sol­ prepared for testing in accordance with ubilize the sample. If heated, cool STM SSS/77. to room temperature before titrating. Titrate the sample with O.lOOON 5. 'h1r.1BER OF DETERMINATIONS aqueous HCL and determine the volume(V) of titrant consumed from the S-shaped In most cases the test can be run as a titrationcurve. Carry out a blank single determination. determination (Vb) using only the 25 ml of solvent. 6. APPARATUS beaker

- 50 ml 

## (disposable) potentiograph (!-fetrohm E536 or equivalent) 5 t::ll buret micro-combination pH electrode magnetic stirrer magnetic stirring bar balance

- accurate to 

## + O.OOlg 50 ml repipet**dispense~** 

## cover glass

- 50 mID =ORM 3561 5·77 

### Page 2'fJ

## 51 :'ivA/80**?dg~** 

## 2
9. 

## C;..LCt-"LATIONS**~!eo** 

## . 

## of .Base**~EQ** 

# = (V

- Vb) 

## x (0.1000) S\{



## ...·here: V 

# = volume of O.lOOON HCL 

## in ml 

## used for titration V 

## = 

## volume of O.lOOON HCL 

## in m1 uged for blank S = 

## sample weight in grams

w


## •Base Number B.V. 

# = (V

- Vb) x 

## (0.1000) x 

## 56.1 Sw OR 

## B.V. = 

## MEQ of Base x 56.1 10. 

## ?RECISION Actual precision data for this micro**~ethod** 

## have not yet been produced;**~o~ever,** 

## precision should be similar to that for the standard method which is: Repeatability 

## = 

# ± 3% Reproducibility = 

## + 

## 5% 11.**~EPORT** 

## OF ANALYSIS 7he report shall contain the test =ethod employed, the result and any changes or unusual observations. 12.**::\EFERE~CES**



# . sr.·! 361D 

## 13. NOTES 

## A. If a potentiograph is not available, this method can be run, using the proper indicator. Recommended indicators include phenol red, phenolphthalein and thymol blue. When choosing an indicator, the strength of the base species be considered. However, it should be noted that a potentiographic endpoint is the only universal endpoint. 

## B. Samples which are not soluble in the PG/THF mixture can be run using a suitable solvent assuming the replacement solvent does not interfere With the test and a blank is run• 

## 14. AUTHOR AND DATE**_w~~** 

## September 18. 1980 

## lela

Page 

## 26:"

_ c 

## Detennination ofWater Content by Catalyzed 

## Karl FISCher TItration 

## STANDARD TESTING METHOD 12/89

CAUTION: Personnel using this method should be 

## familiar with safety and handling precautions for both the material tobe 

## tested and the reagents used 

## in 

## the testing method. 1. Scope 1.1 This method is applicable for the determination ofFREEwater and the water of hydration in most solid or liquid organic and inorganic compounds. 1.2 This method is not applicable to most aldehydes, reactive ketones, strong amines, mercaptans or compounds which are subject to oxidation-reduction reactions in an iodine-iodide system. Common interferences are listed in Table 1 

## 1.3 This method is suitable for the measurement ofwater over a concentration range of 

# oto 10 percent by weight. 1.4 Materials which have a water content greater than 10 percent are analyzed following Standard Testing Method 54/89. 1.5 The water content of amines is determined following Standard Testing Method 96/89. 1.6 The water content ofsolids samples which are insoluble in the recommended solvent system or viscous materials are analyzed following Standard Testing Method 78/90. 2. Summary ofMethod 2.1 In this method a specimen ofthe material to be analyzed is dissolved or dispersed in pyridine, or another appropriate solvent (Note 13.1), and titrated directly with standardized Karl Fischer reagent. 2.2 Karl Fischer reagent is a mixture of iodine, sulfur dioxide, pyridine, and methanol or glycol ether. In the reaction with water, the iodine is reduced to colorless hydrogen iodide. This reaction continues as long as water is present in the reaction system. 2.2.1 CsHsN '12 

# + CsHsN 'S02 

# + CsHsN 

# + H2 0 -+ 

## 2CsHsN 'HI 

# + CsHsN 'S03 2.2.2 CsHsN 'S03 

# + ROH -+ 

## CsHsN " HS04

## R 2.3 When the reaction is complete, the appearance of free iodine in the system is detected electrometrically via a platinum electrode and the titration is stopped. 2.4 The sluggish reaction ofwater with Karl Fischer reagent in pyridine is accelerated using a chemical catalyst, 1-ethylpiperidine.

FORM 3961 '·83 

## Page 27

## STM 12/89 

## Page 2
3. Safety 3.1 Chemicals employed in this method and samples tested by this method may be toxic and/or corrosive. Adequate eye protection must be worn while using this procedure and gloves must be worn where applicable. 3.2 All work must be performed in a fume hood. 3.3 

## Karl Fischer reagent contains four toxic components, iodine, sulfur dioxide, pyridine, and methanol or glycol ether. Care must be exercised to avoid skin contact with or inhalation ofthis reagent system. 3.4 The catalyst, 1-ethylpiperidine, is ofunknown toxicity and therefore must be handled with the same care as the Karl Fischer reagent. 4. Sampling 4.1 All sampling shall be performed in accordance with Standard Testing Method SS/83. 4.2 The sample shall be prepared for testing in accordance with Standard Testing Method SSS/83. 5. Related Methods 5.1 Standard Testing Method 96/89, "Determination ofthe Water Content of Organic Bases". 5.2 Standard Testing Method 54/89, "Determination of the Water Content ofWater Borne Coatings". 5.3 Standard Testing Method 78/90, "Determination ofthe Water Content ofViscous Materials". 6. Apparatus 6.1 Analytical balance, accurate to 0.1 mg. 6.2 Glass dropping bottles, Fisher Scientific, Catalog No. 02-983A (Note 13.2). 6.3 Karl Fischer titrator, Metrohm 658 or equivalent. 6.4 Medicine droppers.

Page 28

## /- ./



## STM 12/89 

## Page 3 6.5 Plastic syringes, Fisher Scientific, Catalog No. 14-823-38 and 14-823-140. 6.6 Plastic transfer pipets. 6.7 Repipetor, 5 or 10 mL for l-ethylpiperidine. 6.8 Repipetor, 50 mL for pyridine. 6.9 Scintillation vials, 20 mL glass. 6.10 Syringe, 100 microliter. 7. Reagents 7.1 Butyl cellosolve, purified. 7.2 Dimethylformamide, reagent grade. 7.3 Distilled or deionized water. 7.4 l-Ethylpiperidine, reagent grade. 7.5 Karl Fischer reagent, Fisher Scientific Company, Catalog No. SK3. 7.6 Methanol, reagent grade. 7.7 Pyridine, reagent grade. 7.8 Tetrahydrofuran, reagent grade. 

## 8. Procedure 8.1 Standardization of Karl Fischer reagent. 8.1.1 Add enough fresh pyridine into the reaction vessel to cover the electrode tip and start the stirring unit. 8.1.2 Add 1 mL of l-ethylpiperidine per 19 mL of pyridine in the reaction vesseL The catalyst performs best at a concentration of5% of the volume present in the reaction vessel. 8.1.3 Pre-titrate the pyridine/l-ethylpiperidine mixture to the endpoint indicated by the instrument manufacturer. Most automatic titrators will dispense to a preset endpoint, adding enough Karl Fischer reagent to yield an endpoint which is stable for thirty seconds (Note 13.3, Attachment 

## I).

Page 29/ 

## /.­

STM 12/89 

## Page 4
8.1.4 Fill the 100 microliter syringe approximately 75 percent full with distilled or deionized water. Weigh the syringe and water and record the weight, A 

## 8.1.5 Empty the contents ofthe syringe into the titration vessel and immediately start the titration. Re-weigh the syringe and record the weight, 

## B. 8.1.6 Upon completion ofthe titration, record the volume ofKarl FISCher reagent used in mL, V, and calculate the standardization factor following Section 9.1 (Note 13.4). 8.1.7 Upon completion ofa single analysis, discard the spent solvent and thoroughly rinse the electrode, delivery tubes, and reaction vessel with methanol and dry. 8.1.8 Repeat Section 8.1.1 to 8.17 for the duplicate analysis. 8.1.9 The duplicate values must agree to within 1% relative, ifnot, discard the data and repeat the standardization. 8.1.10 The Karl Fischer reagent must be re-standardized weekly orwhenever fresh reagent is added to the reservoir. 8.2 Analysis ofsamples containing less than 10% water. 8.2.1 Add enough fresh pyridine into the reaction vessel to cover the electrode tip and start the stirring unit. 8.2.2 Add 1 mL of l-ethylpiperidine per 19 mL ofpyridine in the reaction vessel. The catalyst performs best at a concentration of5% of the volume present in the reaction vessel. 8.2.3 Pre-titrate the pyridine/l-ethylpiperidine mixture to the endpoint indicated by the instrument manufacturer. Most automatic titrators will dispense to a pre-set endpoint, adding enough Karl Fischer reagent to yield an endpoint which is stable for thirty seconds (Note 13.3, Attachment 1). 

## 8.2.4 Place a portion ofthe sample into a vial using a transfer pipet (Note 13.2). Weigh the vial, transfer pipet, and sample and record the initial weight, C. 

## 8.2.5 Using Table II as a guide, add the appropriate amount ofspecimen into the reaction vessel.

Page 30

### , 

### ;!1

.. .. 

## /'**r~** 

### , -' ;'.­ 

# , STM 12/89 PageS


## TABLEll TIIEORETICAL % 

## WATER SPECIMEN WEIGIIT. G 

# oTO 0.5 0.5 TO 1.0 1.0 TO 2.0 2.0 TO 4.0 4.0 TO 6.0 6.0 TO 8.0 8.0 TO 10.0 5.0 3.0 

## 1.5 0.75 0.40 

## 0.30 0.20
8.2.6 Stir the specimen until it has completely dissolved or dispersed. Samples which are not soluble in pyridine can be tested by replacing up to 75 percent of the pyridine with a suitable solvent (Note 13.1).
8.2.7 Titrate the specimen with Karl Fischer reagent to the pre-set endpoint. Record the volume ofKarl Fischer reagent used to titrate the specimen in mL, T. 8.2.8 Reweigh the vial, transfer pipet and remaining specimen and record the final weight, D. , 8.2.9 Calculate the water content ofthe sample following Section 9.2. 8.2.10 Repeat Sections 8.2.5 to 8.2.9 for the duplicate sample analysis. 8.2.11 Upon completion ofthe duplicate analyses, discard the spent solvent and thoroughly rinse the electrode, delivery tubes, and reaction vessel with methanol and dry (Note 135). 8.2.12 Replace the spent solvent with fresh pyridine and 1-ethylpiperidine for use in the next sample analysis. Optimum results are obtained with fresh reagents, that is, no previously titrated specimen present in the reaction vessel. 8.3 Upon completion of all analyses, drain the spent solvent and thoroughly rinse the electrode, delivery tubes, and reaction vessel with methanol and dry. Refill the reaction vessel with pyridine (Note 13.6).

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# , " 

## 81M 12/89 Page 6
9. Calculations 9.1 The Karl Fischer reagent titer is equal to; 9.1.1 Factor (F) 

# = (A-B) x 1000 V 

## where: A 

# = Initial syringe weight g, Section 8.1A. 

## B = 

## Final syringe weight g, Section 8.1.5. V 

## = Volume ofKarl Fischer reagent titrated, mL Section 8.1.6. and 1000 is the conversion factor for grams into milligrams. 9.2 The weight percent water in the sample is equal to; 9.2.1 

## % Water 

# = F x T x 100 (C-D) x 1000 where: 

## F = 

## Standardization factor, mglmL, Section 9.1. 

## T 

# = Volume ofKarl Fischer reagent used to titrate the specimen, mL, Section 8.2.7. C = 

## Initial weight ofthe vial, sample, and transfer pipet, g, Section 8.2.4. D 

# = Final weight ofthe vial, sample, and transfer pipet, g, Section 8.2.8. and 1000 is the conversion factor for grams into milligrams and 100 is 

## the conversion factor for weight percent. 10. Report ofAnalysis 10.1 The report shall contain the test method number and the average ofthe duplicate determinations.

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# /!!: /**f:~-** 

## /.­

,. 

## STM 12/89 Page 7
11. Precision 11.1 Over a concentration range of0 to 10 percent water, duplicate analyses should agree to within 2.0 percent relative. 11.2 The relative standard deviation over the concentration range of0 to 10 percent water is: 11.2.1 0 to 0.1% water, 13.8% relative. 11.2.2 0.1 to 1.0% water, 1.6% relative. 11.2.3 1.0 to 5.0% water, 1.3% relative. 11.24 5.0 to 10.0% water, 1.2% relative. 12 References 12.1 ASTM Standard Test Method D4017-81, "Water in Paints and Paint Materials by 

## Karl Fischer Method", 12.2 ASTM Standard Test Method E203..64, "Water Using Karl Fischer Reagent". 13. Notes 13.1 The addition of a co-solvent into the reaction vessel will often aid in sample solubilization. The solvent must be inert to both the sample and the 

## Karl Fischer reagent. Suitable solvents would include methanol, dimethylformamide, methylene chloride, tetrahydrofuran, butyl cellosolve, and toluene. 13.2 In addition to glass vials and plastic transfer pipets, disposable plastic syringes or glass or plastic dropping bottles are useful for both specific and routine sample analysis. The use ofsealable sample containers is recommended for the analysis ofvolatile compounds, odorous samples, hygroscopic, and toxic materials. 13.3 The recommended time delay for most titrations' endpoints is thirty seconds. Instruments which are set up in laboratory fume hood are subject to increased exposure to atmospheric moisture which may result in endpoint drift. The endpoint time delay may be optimized to account for the drift. Reset the time delay for 10 to 15 seconds. In addition, the use ofthe 1-ethylpiperidine catalyst increases the reaction rate ofwater with Karl Fischer reagent. A stable endpoint with little or no endpoint drift is obtained in a reduced time, reducing the need for an extended endpoint time delay (30 seconds).

Page 33/ 

## /­
,/ 

## STM 12/89 PageS
13.4 Most Karl Fischer titrators are capable ofcalculating both the standardization factor and the water content ofthe sample. Ifso equipped, enter both the sample code and weight for documentation.
13.5 The reaction**vesse~** 

## electrode, and delivery tubes can 

## be cleaned with any solvent which will remove resin residue. After thorough cleaning, rinse all parts with a final methanol rinse. Pigment residue may 

## be removed with a soft cloth. The electrode may be cleaned by immersion into concentrated hydrochloric acid (37%) for one minute followed by a rinse 

## with distilled water then methanol. 13.6 Do not allow the electrode to remain in a solvent solution which contains titrated resin and/or pigment. These materials may coat the electrode and reduce its sensitivity. In addition, do not store the electrode in a pyridine solution which contains the catalyst, as this amine will decompose upon long-term exposure to light
12 Author and Date

January. 1990 Attachment

Page 34/ 

# 17/ /-­

, ,,­ <


## TABLE I
COMPOUNDS AND ClASSES OF COMPOUNDS WInCH REACf WfI1I 

## KARL FISCHER REAGENT, STOICHIOMEIRICALL Y: ASCORBICACID HYDRAZINE 

## DERN ATIVES MERCAPTANS SILANOLS,**~iOH** 

## AND**~Si(OH)2** 

## ARSENATE, RAs04 

## ARSENITE, RAs0

## s BORICACID BORIC OXIDE BICARBONATES CUPRIC SALTS FERRIC SALTS MEfALHYDROXIDES MEfAL OXIDES, 

## Cao, MgO, ZnO, Ag20, HgO,

# CuzO, Mn02 ' PhO, Pb02 PYROSULFlTES 

## SODIUM NITRATE SULFlTES 

## STANNOUS SALTS TEfRABORATE TIIIOSULFATE TIIESE COMPOUNDS REACf ONLY PARTIALLY WITII KARL FISCHER REAGENT: MEfHYLOLUREA PEROXIDES QUINONES ARSENIOUS OXIDE CHROMATES DICHROMATES mONOXIDE NICKEL OXIDE 

## VINYLEmYL EmER DI KETOAMINES ALDEHYDES FORMICACID STRONG AMINOS KETONES

Page 35**~-t;** .•**~**

. 

## ,.**f~·** 

# ,. ATTACHMENT I: 1ITRATION PARAMEIERS FOR MEIROHM 6581TIRATOR
KF: PARAMEIER 

## REPORT 658 

## DATE: 89-07-24 

## TIME: 13:35 

## REF. NO. 003.70091 

## SIOP 

## DElAY 10 S KFR TIlER 6.714MGIML BLANK O.MG BACKTI'IER 0.000 

## MG/ML KFR

## VOLUME O. 

## ML EX.TR. 

## TIME 0 MIN 

## SOLVENT 0.00 

## ML FAcroR 1 REPORTMODE: M. 

## FRAC, MEAN, SHORTCOpy END MODE: CONDmONING

- BUZZER ON

IN ADDmON ON TIlE655 DOSIMAT SETTIlESTIRRING SPEED ON3 AND SETTIlE DOSING SPEED, dV/dt (VOLUME EXPELLED V PER TIME

## t), ON2 THISDOSING SPEED IS RECOMMENDED FOR BornTIlESTANDARDIZA1l0N ANDTIlEANALYSIS OFALL SAMPLES WIllCH CONTAIN 1PERCENTWATER ORMORE. WHEN TIlEWATER CONTENT OFTIlE SAMPLE IS LESS mAN 

## 1PERCENT «1%), SET TIlEDOSING SPEEDTO 1 TO AVOID OVER-1ITRA1l0N.

Page 36