~r---~-------------------------------------------------------------------------------~ 

N 

ANY SAl\l\1IZED~ S? 

Form Approved. O.M.B. No. 2070-0012. Approval Expires 10-31-96. 

U. S. ENVIRONMENTAL PROTECTION AGENCY ~,~4MENCY US~ONLY

Date ofreceipC' ,,'

PREMANUFACTURE &EPA NOTICE rn 39 .'

..,­ FOR NEW CHEMICAL SUBSTANCES ;::~ 

\\ 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 


Enter the total number of pages 


in the Premanufacture Notice 


GENERAL INSTRUCTIONS 

·You must provide all information requested in this form to the extent that it is known to or reasonably ascertainable by you. Make reasonable estimates if you do 

not have actual data• 

•Before you complete this form, you should read the "Instructions Manual for Premanufacture Notification" (the Instructions Manual is available from the Toxic 

Substances Control Act (TSCA) Information Service by calling 202-554-1404, or fadng 202-554-5603). 

·If a user fee bas been remitted for this notice (40 CFR 700.45), indicate in the boxes above the TS-user fee identification number you have generated. 

Remember, your user fee ID number must also appear on your corresponding fee remittance, which is sent to: EPA, HQ Accounting Operations Branch (PM-266), 

P.O. 360399M, Pittsburgh, PA 15251-5399, Attn: TSCA User Fee. 

Part I-GENERAL INFORMAnON 

You must provide the currently correct Chemical Abstracts (CA) Name ofthe 

new chemical substance, even if you claim the identity as confidential. You may 

authorize another person to submit chemical identity information for you, but 

your submission will not be complete and review will not begin until EPA 

receives this information_ A letter in support of your submission should 

reference your 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 be submitted. 

Part II-HUMAN EXPOSURE AND ENVIRONMENTAL RELEASE 

If there are several manufacture, processing, or use operations to be described in 

Part 11, sections A and B ofthis notice, reproduce the sections as needed. 

Part III-LIST OF ATTACHMENTS 

Attach additional sheets ifthere is not enough space to answer a question fully. 

Label each continuation sheet with the corresponding section heading. In Part 

III, list these attachments, any test data or other data and any optional 

information included in the notice. 

OPTIONAL INFORMATION 

You may include any information that you wnat EPA to consider in evaluating 

tbe new 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 for you to indicate 

your willingness to be bound to certain statements you make in this notice, such 

as use, Jlroduction volume, protective equipment. .. This option is intended to reduce delays that routinely accompany the development of consent orders or 

Significant New Use Rules. Except in the case of exemption applications (such as 

TMEA, LVE, LOREX) where certain information provided in such notification is 

binding on the submitter when the Agency approves the exemption application, 

checking a binding box in this notice dm.n!tt by itself prohibit the submitter 

from later deviating from the information (except chemical identity) reported in 

the form. 

CONFIDENTIALITY CLAIMS 

You may claim any information in this notice as conrldential. To assert a claim 

on the form, ma rk (X) the confidential box next to the information that you claim 

as conrldential. To assert a claim in an attachment, circle or bracket the information 

you claim as confidential. I f you claim information in the potice as 

confideptial you must nrovide a sapitized version ofthe potice. ipcluding 

attachments), For additional instructions on claiming information as 

confidential, read the Instructions Manual. 

Mark (X) if any information in this notice is claimed as confidential 

TEST DATA AND OTHER DATA 

You are required to submit all test data in your possession or control 

and to provide a description of all other data known to Or reasonably 

ascertainable by you, if these data are related to tbe health and 

environmental effects of the manufacture, processing, distribution 

in commerce, use, or disposal of the new chemical substance. Standa rd 

literature citations may be submitted for data in the open scientific 

literature. Complete test data (written in English), not summaries ofdata. 

must be submitted if thev do not anpear in the onen literature, You should 

clearly identify whether test data is on the substance or on an analog. Also, 

the chemical composition of the tested material should be characterized. 

Following are examples of test data and other data. Data should be 

submitted according to the requirements of §720.50 of the Premanufacture 

Notification Rule (40 CFR Part 720). 

Test Data (Check Below any included in this notice) 

• Environmentalfatedata 0 Yes • Other Data 0 Yes 

• Health effects data 0 Yes 	 Risk assesments 

• Environmental effects data 0 Yes 	 Structure/activity relationships 

• PhysicaVChemical Properties • 	 Test data not in the possession 

Or control ofthe submitter 

•A physical and chemical properties worksheet is located on the last page 

of Ibis form. 

TYPE OF NOTICE (Check Only One) 

PMN (Premanufacture Notice) 

INTER MEDIA TE PMN (submitted in sequence with final product 

PMN) 

o SNUN (Significant New Use Notice) 

o TMEA (Test Marketing Exemption Application) 

o LVE (Low Volume Exemption) • CFR 723.50 (c)(l) 

o LOREX (Low ReleaseILow Exposure Exemption)' 723.50(c)(2) 

o 	LVE Modification o Lore" Modification

IS THIS A CONSOLIDATED PMN? [8J Yes 

II- of chemicals 3 

(Prenotice Communication II- required, enter II- on page 3) 

EPA FORM 7710-25 (Rev. 5-95) 	 Replaces previous editions ofEPA Form 7710-25 
Public reporting burden for this collection of information is estimated to average 110 hours per response, including time for reviewing instructions, 

searching existing data sources, gathering and maintaining the data needed, and completing and reviewing the collection of information. Send 

comments regarding the burden estimate or any other aspect 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 of my knowledge and belief: 

I. The company named in Part I, section A, subsection I a of this notice form intends to manufacture or import for a 

commercial purpose, other than 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 of the date of submission. 

3. I am submitting with this notice all test data in my possession or control and a description of all other data known to 

or reasonably ascertainable by me as required by §720.50 of the Premanufacture Notification Rule. 

Additional Certification Statements: 

If you are SUbmitting a PMN, Intermediate PMN, Consolidated PMN, or SNUN, check the following user fee certification 

statement that applies: 

The Company named in Part I, Section A has remitted the fee of $2500 specified in 40 CFR 700.45 (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). 

If you 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 CFR 723.50 (c) (2), check the 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 

of 40 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. 

If this application is for an LVE in accordance with 40 CFR 723.50 (c)(I), the manufacturer intends to commence 

manufacture of the exempted substance for commercial purposes within 1 year of the date ofthe expiration of the 

30 day review period. 

The accuracy of the statements you make in this notice should reflect your best prediction of the anticipated .Ca~ chemical 

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

~&A Confidential 

Signature and title of Authorized Official (Original Signature Required) Date 

Signature of agent - (if applicable) Date 

FORM EPA 7710-25 (Rev. 5-95) Page 2 
Part I -- GENERAL INFORMATION 

Section A -- SUBMITTER IDENTIFICATION 

~------------------------------------------------------------------------------------~ 

Confidential 

Mark (X) the "Confidential" box next to 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 part of ajoint submission, mark (X) this box. 

Ioint 

Submitter 

(if applicable) 

2. Technical 

Contact 

(in U.S.) 

Name 

you or 

import for the chemical substance covered by this notice, enter the 

notice number assigned by EPA. 

Mark (X) 

if none D 

Mark (X) 

if none 

Mark (X) 

if none • 

6. Type of Notice -- Mark (X) l. 

D Binding Option 

Mark (x) 

2. 

D Binding Option 

Mark (x) 

3. Both 

FORM EPA 7710·25 (Rev. 5-95) Pagel 
Part I -- GENERAL INFORMATION -- Continued 

You must provide a currently correct Chemical Abstracts (CA) name of the substance Section B - CHEMICAL IDENTITY INFORMATION based on the ninth Collective Index (9<:1) of CA nomenclature rules and conventions. 

Complete either item 1 (Class 1 or 2 substances) or 2 (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 at the right 

IdentifY the name, company, and address of that person in a continuation sheet. ... 0 

I. 	 Class 1 or 2 chemical substances (for definitions 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 correct Chemical Abstracts (CA) Name that is consistent with TSCA Inventory listings for similar substances. 

For Class I substances a CA Index Name must be provided. For Class 2 substances either a CA Index Name or CA Preferred Name must 

be provided, whichever is appropriate based on CA 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 of the Identification 

~ report obtained from the CAS Inventory Expert Service must be 

submitted as an attachment to this notice) 

o Method 2 (Other Source) 

d. Molecular formula and CAS Registry Number (if a number already exists for the substance) 

CAS# 

e. For a class 1 substance, provide a complete and correct chemical structural diagram. For a class 2 substance - (I) List the immediate 

precursor substances with their respective CAS Registry Numbers. (2) Describe the nature of the reaction or process. (3) Indicate the 

range of composition and the typical composition (where appropriate). (4) Provide a correct representative or partial chemical 

structural diagram, as complete as can be known, if one can be reasonable ascertained. 

o Mark (X) this box if you attach a continuation sheet. 
Part I -- GENERAL INFORMATION -- Continued 

You must provide a currendy correct Chemical Abstracts (CA) name of the substance Section B -- CHEMICAL IDENTITY INFORMATION based on the ninth Collective Index (9CI) ofCA nomenclature rules and conventions. 

Complete either item 1 (Class 1 or 2 substances) or 2 (Polymers) as appropriate. Complete all other items. 

Ifanother person will submit chemical identity infonnation for you (for either item I or 2), mark (x) the box at the right. 

Identii}' the name, company, and address of that person in a continuation sheet. • 0 

I. 	 Class 1 or 2 chemical substances (for definitions of class I and class 2 substances, see the Instructions Manual) 

a. 	 Class of substance - Mark (X) 1 [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. 

For Class I substances a CA Index Name must be provided. For Class 2 substances either a CA Index Name or CA Preferred 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 of the Identification Method 2 (Other Source) 


report obtained from the CAS Inventory Expert Service must be 


submitted as an attachment to this notice) 


d. 	 Molecular fonnula and CAS Registry Number (if a number already exists for the substance) 

CAS# 

e. For a class 1 substance, provide a complete and correct chemical structural diagram. For a class 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 of composition and the typical composition (where appropriate). (4) Provide a correct representative or partial chemical 


structural diagram, as complete as can be known, if one can be reasonable ascertained. 


D Mark (X) this box if you attach a continuation sheet. 
Part I - GENERAL INFORMATION -- Continued 

You must provide a currently correct Cbemical AbstracD (CA) name of tbe substance Section B -- CHEMICAL IDENTITY IN FORMATION based on the nintb Collective Index (9CI) of CA nomenclature rules and conventions. 

Complete either item 1 (Class 1 or 2 substances) or 2 (Polymers) as appropriate. Complete all other items. 

If another person will submit chemical identity information for you (for either item I or 2), mark (x) the box at the right. 


IdentitY the name, company, and address ofthat person in a continuation sheet. ---....... 0 


I. 	 Class 1 or 2 chemical substances (for definitions of class I and class 2 substances, see the Instructions Manual) 

a. 	 Class of substance -- 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. 

For Class 1 substances a CA Index Name must be provided. For Class 2 substances either a CA Index Name or CA 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 or obtain the specified chemical identity information reported in this notice: 


(check One). 


D Method 1 (CAS Inventory Expert Service - a copy of the 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 (if a number already exists for the substance) 

CAS# 

e. For a class 1 substance, provide a complete and correct chemical structural diagram. For a class 2 substance - (I) List the immediate 

precursor substances with their respective CAS Registry Numbers. (2) Describe the nature of the reaction or process. (3) Indicate the 

range of composition and the typical composition (where appropriate). (4) Provide a correct representative or partial chemical 

structural diagram, as complete as can be known, if one can be reasonable ascertained. 

D Mark (X) this box if you attach a continuation sheet. 
Part I -- GENERAL INFORMATION -- Continued 

~ Section B - CHEMICAL IDENTITY INFORMATION -- Continued 

2. Polymers (For a definition of polymer, see the Instructions Manual.) ;:~r~1 a. Indicate the number-average weight ofthe lowest molecular weight composition ofthe polymer you intend to manufacture. 

Indicate maximum weight percent oflow molecular weight species (not including residual monomers, reactants, or solvents) below 

500 and below 1,000 absolute molecular weight ofthat composition. 

Describe the methods of measurement or the basis for your estimates: 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 if you attach a continuation sheet. 

b. You must make separate confidentiality claims for monomer or other reactant identity, composition information, and residual information. 

Mark (X) the ·Confidential" box next to any item you claim as confidential. 

(I) -- Provide the specific chemical name and CAS Registry Number (if a number exists) of each monomer or other reactant used in the 

manufacture of the polymer. 

(2) -- Mark (X) this column if entry in column (I) is confidential. 

(3) - Indicate the typical weight percent ofeach monomer or other reactant in the polymer. 

(4) -- Mark (X) the identity column if you want a monomer or other reactant used at two weight percent or less to be listed as part of the 

polymer description on the TSCA Chemical Substance Inventory. 

(5) -- Mark (X) this column if entries in columns (3) and (4) are confidential. 

(6) -- Indicate the maximum weight percent ofeach monomer or other reactant that may be present as a residual in the polymer as 

manufactured for commercial purposes. 

(7) -. Mark (X) this column if entry in column (6) is confidential. 

Monomer or other reactant 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 if you 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 t to this notice) 

d. The currently correct Chemical Abstracts (CA) name for the polymer that is consistent with TSCA Inventory listings for similar polymers. 

e. Provide a correct representative or partial chemical structure diagram, as complete as can be known, if one can be reasonably ascertained. 

0 Mark (X) this box if you attach a continuation sheet. 

FORM EPA 7710-25 (Rev. 5-95) PageS 
Part I -- 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 for commercial purposes. 

Provide the CAS Registry Number iCavaiiable. Ifthere are unidentified impurities, enter "unidentified." 

(b) ­ Estimate the maximum weight "I. of each impurity. If there 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 if you attach a continuation sheet. 

4. Synonyms ­ Enter any chemical synonyms for the new chemical substance identified in subsection 1 or 2. ;:~~:I 

0 Mark (X) this box if you attach a continuation sheet. 

5. Trade identification ­ List trade names for the new chemical substance identified in subsection 1 or 2. 

0 Mark (X) this box if you 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 to the maximum extent possible. 

Refer to the TSCA Chemical 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. 

AJt1tr-t~A 7. ~.H" uu""'" ­ Describe any 't' : resulting from the 'r .!g, use, or disposal of the new chemical • 'v 'A<;: 

Registry Number if available. ·'VI/)~.. Byproduct CAS Registry Number .... -..1'1 

(I) (2) r~1 

None known 

0 Mark (X) this box if you attach a continuation sheet. 

FORM EPA 7710-25 (Rev. 5-95) Page 6 
Part I -- 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 of production. Also estimate the 

maximum production volume for any consecutive 12-month period during the first three years of production. Estimates should be on 

100% new chemical substance basis. For a Low Volume Exemption application. ijyou choose to have your notice reviewed at a lower 

production volume than 10,000 kg/yr, specify the volume and nwrk (x) in the binding box. Ifgranted, you are bound to 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 of the category of use, the percent of production volume 

devoted to each category, the formulation of the new substance, and other use information. Mark (X) the "Confidential" Box next to any item you 

claim as confidential. 

a. (I) -- Describe each intended category of use of the 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 percent of total production for the first three years devoted to each category of use. 

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

(6) - Estimate the percent of the 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 of use. 

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

(8) -- Indicate % of product volume expected for the listed "use" sectors. Mark more than one box if appropriate. Mark 

(X) to indicate your willingness to have the use type provided in (8) binding. 

{O\ __ M",1c {Y\ thi. ""I11mn if, in ""I11mn (I!\ i. (,.....i .Co. • I hll im'••. £rRIi 

Category of use (I) CBI Binding Produc- CBI %in CBI % ofsubstance expected per use 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 

% % 

% % 

% % 

% % 

"'If you have identified a "consumer" use, please provide on a continuation sheet a detailed description of the use(s) of this chemical 

substance in consumer products. In addition include estimates of the concentration of the 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 a continuation sheet. 

b. Generic Ifyou claim any category of use description in subsection 2a as confidential, enter a generic description of tbat use category. Read tbe Instructions Manual for examples of generic 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 a copy of reasonable facsimile of any hazard warning statement, label, material safety data sheet, Binding 

or other information which will be provided to any person who is reasonably likely to be exposed to this substance regarding protective Option 

equipment or pl1lctices for the safe handling, transport, use, or disposal ofthe new substance. List in part III hazard 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 
Part II -- HUMAN EXPOSURE AND ENVIRONMENTAL RELEASE 

Section A -- INDUSTRIAL SITES CONTROLLED BY THE SUBMITTER 

Mark (X) the "Confidential" box next to any item you 

claim a. c:onfidential 

ofthe site at which the will occur. 

Mark (X) this box if you attach a continuation sheet. 

o Processing o Use 

Hourslbatch Batches/year 

substance) 24 12 

,V'."'IU"UlU kg/day (100% new chemical Hours/day Days/year 

substance) 

Mark (X) to indicate your willingness to have your process description binding. 

(\) Diagram the 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 or kglbatch, on a 100% new chemical substance basis), and entry point of all starting 

materials and feedstocks (including reactants, solvents, and catalysts, etc.), and of all produets, recycle streams, and wastes. Include cleaning 

chemicals (note frequency if not used daily or per batch.). 

(3) Identify by number the points ofrelease, including small or intermittant releases, to the environment of the new chemical substance. 

Please see Page 8A1 

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

Confidential 
Continuation Sheet for Part II. Section A. Item lid - Process Description 

Page 8AI 
Continyation Sheet for Part II. Section A. Item 1 (d) 

Process Description 

Page 8A2 
Continuation Sheet for Part II. Section A, Item 1(d) 

Process Description 

Page SA3 
Section A -- INDUSTRIAL SITES CONTROLLED BY THE SUBMITTER 

you 

If the same operation will occur at more than one site, enter the number of sites. Identify the 

additional sites on a continuation sheet, and if any of the 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 if you attach a continuation 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. 5 gallon pails, 55 

gallon drum, rail car, tank truck, etc.). 

(2) Provide the identity, the approximate weight (by kg/day or kglbatch, on a 100% new chemical substance basis), and entry point of all starting 

materials and feedstocks (including reactants, solvents, and catalysts, etc.), and of all products, recycle streams, and wastes. Include cleaning 

chemicals (note frequency if not used daily or per batch.). 

(3) Identify by number the points of release, including small or intermittant releases, to the environment of the new chemical substance. 

o Mark (X) this box if you attach a continuation sheet. 

Part II -- HUMAN EXPOSURE AND ENVIRONMENTAL RELEASE 

Mark (X) the "Confidential" box next to any item you 

claim a, confidential 

each type of manufacture, or use new 


Importers do not have to complete this section for operations outside the U.S.; however, you may still have reporting requirements if there are 


further industrial processing or use operations after import. You must describe these operations. See instructions manual. 


Confiof the site at which the will occur. dential 

(number and street) 
Part II -- HUMAN EXPOSURE AND ENVIRONMENTAL RELEASE 

Section A -- INDUSTRIAL SITES CONTROLLED BY THE SUBMITTER 

Mark (X) Ihe "Confidential" OOX next to any item you 

claim as confidential 

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 if there are 

further industrial processing or use operations after import. 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 your willingness to have your process description binding. 

6 

(1) Diagram the major unit operation steps and chemical covers ions. 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 or kglbatch, on a 100% new chemical substance basis), and entry point of all starting 

materials and feedstocks (including reactants, solvents, and catalysts, etc.), and of all 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 intermittant releases, to the environment of the new chemical substance. 

D Mark (X) this box if you attach a continuation sheet. 

Coofi· 

dentiaI 

number ofsites. # ofsites

Mark (X) this box if you attach a continuation sheet. 
Part II -- 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 of worker activity, physical form of the new chemical 

substance, number of workers exposed, and duration of activity. 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, or dust) and % new chemical substance (if part of 

a mixture) at the time of exposure. 

(7) -- Mark (X) this column if entry in column (5) is confidential business information (CBI). 

(8) .. Estimate the maximum number of workers involved in each activity for all sites combined. 

(9) •• Mark (X) this column if entry in column (8) is confidential business information (CBl). 

(10) and (II) _. Estimate the maximum duration of the activity for any worker in hours per day and days per year. 

(121 .. Mark (X) thi~ colnmn if entrie 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 Page 90 80-99% 3 0.5 12 

Liquid 

Process samples in lab Please see Page 90 80-99% 3 1.0 12 

Liquid 

Filtration and filling Please see Page 90 95-998

/. 3 1.0 12 

Liquid 

Cleaning equipment Please see Page 90 80-99% 3 0.5 12 

Cbarging Intermediate Stage PMN Liquid 

substance to reactor Please see Page 90 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 of the 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 of each release point identified in the process description, part II, section A, subsection I d(3). 

(2) •• Estimate the amount of the new substance released (a) directly to the environment or (b) into control technology (in kg/day or kglbatch). 

(3) -- Mark (X) this column if entries in columns (I) and (2) are confidential business information (CBI). 

(4) --IdentifY the media of release i.e. stack air, fugitive air (optional-see Instruction Manual), surface water, on-site or off site land or incineration, 

POTW, or other (please specifY) to which the new substance will be released from that release point. 

(5) ­ a. Describe control technology, if any, 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 of RCRA 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 or tertiary on-site treatment. b. Estimate the amount released to the environment after control technology (in kg/day). 

(6) - Mark (X) this column if entries in columns (4) and (5) are confidential business information (CBI). 

(7) -- IdentifY the destinations(s) ofreleases to water. Please supply NPDES (National Pollutant Discharge Elimination System) numbers for direct 

dischargers or NPDES numbers ofthe POTW (publicly Owned Treatment Works). Mark (X) if the POTW name ofNPDES # is confidential h". ,np« • '.{rRH 

Release Amount ofnew substance CBI Media of 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 Pape 9E 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 
Part II -- 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 of worker activity, physical form ofthe new chemical 

substance, number of workers exposed, and duration of activity. 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 if entry in column (1) 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, or dust) and % new chemical substance (if part of 

a mixture) at the time ofexposure. 

(7) -- Mark (X) this column if entry 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 if entry in column (8) is confidential business information (CBI), 

(10) and (11) -- Estimate the maximum duration ofthe activity for any worker in hours per day and days per year. 

(12) -- Mark (X) thi~ column if entrie : 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) {I2) 

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 Page 9D 6-100/0 2 1.0 8 

Liquid 

Cleaning equipment Please see Page 9D 6-10% 2 0.5 8 

D Marie (X) this box if you attach a continuation sheet. 

3. Environmental Release and Disposal -- You must make separate confidentiality claims for the release number and the amount of the 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 of each 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 or leglbatch). 

(3) - Marie (X) this column if entries in columns (1) and (2) are confidential business information (CBI). 

(4) -- Identity the media of release i.e. stacie air, fugitive air (optional-see Instruction Manual), surface water, on-site or offsite land or incineration, 

POTW, or other (please specity) 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 limit the release of the new substance to the environment. 

For releases disposed of on 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 or tertiary 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) - Identity the destinations(s) ofreleases to water. Please supply NPDES (National Pollutant Discharge Elimination System) numbers for direct 

dischargers or NPDES numbers ofthe POTW (Publicly Owned Treatment Worles). Marie (X) if the POTW name ofNPDES # is confidential 

(rRf) 

Release Amount ofnew substance CBI Media of 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) 

(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 Palle 9F 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 if you 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 of actual exposure is estimated at one hour per each reactor, based 

on the fact that most of the 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 Sheet for Part II. Section A, Item 3 


Control Technology for Environmental Release 


Page 9E 
Continuation Sheet for Part II, Section A, Item 3 


Control Technology for Enyironmental Release and Disposal 

Page 9F 
Part II -- HUMAN EXPOSURE AND ENVIRONMENTAL RELEASE -- Continued 

~ Section B ­ INDUSTRIAL SITES CONTROLLED BY OTHERS 

Complete section B for 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 ofprocessing. or use operation involving the new chemical substance. If the 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 bracket the 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, tank trucks, 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 of all products, recycle streams, and wastes. Include cleaning chemicals (note frequency if not used daily or per 

batch). (3) -- Identify by number the points of release, including small or intermittent releases, to the environment of the new chemical substance. 

(4) Please enter the # of sites (remember to identify the locations of these sites on a continuation sheet): 

0 

# of sites 

The subject of this PMN is a chemical intennediate to be used by our company only. It will not be distributed to any 

sites controlled by others. 

0 Mark (X) this box if you attach a continuation sheet. 

2. Worker ExposurelEnvironmental 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 of workers exposed for all sites combined. 

(4) -- Estimate the typical duration of exposure per worker in (a) hours per day and (b) days per year. 

(6) -- Describe physical form of exposure and % new chemical substance (ifin mixture), and any protective equipment and engineering controls, ifany, 

used to protect workers. 

(7) -- Estimate the percent of the new substance as formulated when packaged or used as a final product. 

(9) - From the process diagram above, enter the number ofeach release point. Complete 9-13 for each release point identified. 

(10)- Estimate the amount of the new substance released (a) directly to the environment or (b) into control technology to the environment 

(in kg/day or kglbatch). 

(12) -- Describe media ofrelease (stack air, fugitive air (optional-see Instructions Manual), surface water, on-site or off-site land or incineration, POTW, 

or other (specify» and control technology, ifany, that will be used to limit the 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 a continuation sheet. 

FORM EPA 7710-25 (Rev. 5-95) Page 10 
OPTIONAL POLLUTION PREVENTION INFORMATION 

To claim information in this section as confidential circle or bracket the specific information that you claim as confidential. 

In this section you may provide information not reported elsewhere in this form regarding your 

efforts to reduce or minimize potential risks associated with activities surrounding 

manufacturing, processing, use and disposal of the PMN substance. Please include new 

information pertinent to pollution prevention, including source reduction, recycling activities 

and safer processes or products available due to the new chemical substance. Source reduction 

includes the reduction in the amount or toxicity of chemical wastes by technological 

modification, process and procedure modification, product reformulation, raw materials 

substitution, and/or inventory control. Recycling refers to the reclamation of useful chemical 

components from wastes that would otherwise be treated or released as air emissions or water 

discharges, or land disposal. Descriptions ofpollution prevention, source reduction and 

recycling should emphasize potential risk reduction subsequent to compliance with existing 

regulatory requirements and can be either quantitative or qualitative. The EPA is interested in 

this information to assess overall net reductions in toxicity or environmental releases and 

exposures, not the shifting ofrisks to other environmental media or non-environmental areas 

(e.g., occupational or consumer exposure). In additional, information on the relative cost or 

performance characteristics of the 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 or the 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 of production and/or improved operation efficiency of the new chemical substance in 

comparison to existing chemical substances used in similar applications; or (6) the extent to which the new chemical substance 

may be a substitute for an existing substance that poses a greater overall risk to human health or the 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 Sbeet for Optional Pollution Prevention Information, Page llA 

Page lIB 
Part III - LIST OF ATTACHMENTS 

Attach continuation sheets for sections of the form and test data and other data (including physical! chemical properties and 

structure/activity information), and optional information after this page. Clearly identify the attachment and the section of the form to 

which it relates, if appropriate. Number consecutively the pages of the attachments. In the column below, enter the inclusive page 

numbers of each attachment. 

Mark (X) the "Confidential" box next to any attachment name you claim as confidential. Read the Instructions Manual for 

guidance on how to claim any information in an attachment as confidential. You must include with the sanitized copy of the notice 

form a sanitized version of any attachment in which you daim information as confidential. 

Attachment name Attachment 

page number(s) 

Confidential 

lHazard Warning, Part I, Section c/3 13 

Physicalf Chemical Properties 14 

Intermediate Stage (I) GC 15 

Intermediate Stage (I) IR Spectrum 16 

Intermediate Stage (II) GPC 17 

Intermediate Stage (II) IR Spectrum 18 

Final Product GPC 19 

[Final Product IR Spectrum 20 

Determination of Amine Equivalent Weight Test Method 21-23 

Determination of Hydroxyl Value Test Method 24 

Semi-Micro Determination of Basicity Test Method 25-26 

!Determination of Water Content Test Method 27 -36 

0 Mark (X) this box if you attach a continuation sheet. Enter the attachment name and number. 

FORM EPA 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. A blank 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 N x 14 x 100 


%Am. N2 = ---------------------­ SW X 1000 

Base Number 


(Vs-Vb) X N X 56.1 


Base No. = -----------------­ SW 

%Specific Amine 


%Amine = ___(v s-v __ b 	_______________ ) X N X F X 100
_ 

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. A color 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 titraAce~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.,.ATIONS 


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 equiv11 


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 of basicity 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 

Most 3.0 	 0.05 3.00g 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 

materials. All work 11.2 	 0.20 1.25 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 

with until the 	sample is in solution. In STM SS/77. The sample shall be 

difficult 	cases, heat gently to sol­ prepared for testing in accordance with ubilize the sample. If heated, cool STM SSS/77. 

to room temperature before titrating. 

5. 'h1r.1BER OF DETERMINATIONS Titrate the sample with O.lOOON

aqueous HCL and determine the volume(V) 

of titrant consumed from the S-shaped In most cases the test can be run as a 

titration 	curve. 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: 
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_ c 

Detennination of Water 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 to be tested and the reagents used in the testing method. 

1. Scope 

1.1 	 This method is applicable for the determination of FREE water 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 of water 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 of solids samples which are insoluble in the recommended solvent 

system or viscous materials are analyzed following Standard Testing Method 78/90. 

2. 	 Summary of Method 

2.1 	 In this method a specimen of the 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 + H20 -+ 2CsHsN 'HI + CsHsN 'S03 

2.2.2 	 CsHsN 'S03 + ROH -+ CsHsN " HS04R 

2.3 	 When the reaction is complete, the appearance of free iodine in the system is detected 

electro metrically via a platinum electrode and the titration is stopped. 

2.4 	 The sluggish reaction of water 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 of this reagent system. 

3.4 	 The catalyst, 1-ethylpiperidine, is of unknown 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 of the Water Content of Organic 

Bases". 

5.2 	 Standard Testing Method 54/89, "Determination of the Water Content of Water 

Borne Coatings". 

5.3 	 Standard Testing Method 78/90, "Determination of the Water Content of Viscous 

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 
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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 of 5% 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 
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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 of the syringe into the titration vessel and immediately start 

the titration. Re-weigh the syringe and record the weight, B. 

8.1.6 	 Upon completion of the titration, record the volume of Karl FISCher reagent used 

in mL, V, and calculate the standardization factor following Section 9.1 

(Note 13.4). 

8.1.7 	 Upon completion of a 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, if not, discard the data 

and repeat the standardization. 

8.1.10 	 The Karl Fischer reagent must be re-standardized weekly or whenever fresh 

reagent is added to the reservoir. 

8.2 	 Analysis of samples 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 of pyridine in the reaction vessel. The 

catalyst performs best at a concentration of 5% 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 of the 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 of specimen into the 

reaction vessel. 

Page 30 
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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 of Karl 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 of the 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 of the 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). 

Page 31 
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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 of Karl 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 of Karl Fischer reagent used to titrate 

the specimen, mL, Section 8.2.7. 

C = Initial weight of the vial, sample, and transfer pipet, g, 

Section 8.2.4. 

D = Final weight of the 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 of Analysis 

10.1 	 The report shall contain the test method number and the average of the duplicate 

determina tions. 

Page 32 
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STM 12/89 

Page 7 

11. 	 Precision 

11.1 	 Over a concentration range of 0 to 10 percent water, duplicate analyses should agree to 

within 2.0 percent relative. 

11.2 	 The relative standard deviation over the concentration range of 0 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 

of sealable sample containers is recommended for the analysis of volatile 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 of the 1-ethylpiperidine catalyst increases the reaction rate of water 

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 
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STM 12/89 

PageS 

13.4 	 Most Karl Fischer titrators are capable of calculating both the standardization factor and 

the water content of the sample. If so 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 
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,,­

< 

TABLE I 

COMPOUNDS AND ClASSES OF COMPOUNDS WInCH REACf WfI1I KARL FISCHER 

REAGENT, STOICHIOMEIRICALLY: 

ASCORBIC ACID 

HYDRAZINE DERNATIVES 

MERCAPTANS 

SILANOLS, ~iOH AND ~Si(OH)2 

ARSENATE, RAs04 

ARSENITE, RAs0s 

BORIC ACID 

BORIC OXIDE 

BICARBONATES 

CUPRIC SALTS 

FERRIC SALTS 

MEfAL HYDROXIDES 

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 

FORMIC ACID 

STRONG AMINOS 

KETONES 

Page 35 

~-t; .• ~ 

. ,.f~· 

,. 


ATTACHMENT I: 1ITRATION P ARAMEIERS 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 

BACK TI'IER 0.000 MG/ML 

KFR VOLUME O. ML 

EX.TR. TIME 0 MIN 

SOLVENT 0.00 ML 

FAcroR 1 

REPORT MODE: M. FRAC, MEAN, SHORT COpy 

END MODE: CONDmONING - BUZZER ON 

IN ADDmON ON TIlE 655 DOSIMAT SET TIlE STIRRING SPEED ON 3 AND SET TIlE 

DOSING SPEED, dV/dt (VOLUME EXPELLED V PER TIME t), ON 2 THIS DOSING SPEED 

IS RECOMMENDED FOR Born TIlE STANDARDIZA1l0N AND TIlE ANALYSIS OF ALL 

SAMPLES WIllCH CONTAIN 1 PERCENT WATER OR MORE. 

WHEN TIlE WATER CONTENT OF TIlE SAMPLE IS LESS mAN 1 PERCENT «1%), SET 

TIlE DOSING SPEED TO 1 TO AVOID OVER-1ITRA1l0N. 

Page 36