Epi–dma Polyamines: Awwa Standard

American Water Works Association ANSI/AWWA B452-98 (Revision of ANSI/AWWA B452-90)

R

AWWA STANDARD FOR

EPI–DMA POLYAMINES

Effective date: June 1, 1999. First edition approved by AWWA Board of Directors June 17, 1990. This edition approved June 21, 1998. Approved by American National Standards Institute Jan. 28, 1999.

AMERICAN WATER WORKS ASSOCIATION 6666 West Quincy Avenue, Denver, Colorado 80235

Copyright © 1999 American Water Works Association, All Rights Reserved.

AWWA Standard This document is an American Water Works Association (AWWA) standard. It is not a specification. AWWA standards describe minimum requirements and do not contain all of the engineering and administrative information normally contained in specifications. The AWWA standards usually contain options that must be evaluated by the user of the standard. Until each optional feature is specified by the user, the product or service is not fully defined. AWWA publication of a standard does not constitute endorsement of any product or product type, nor does AWWA test, certify, or approve any product. The use of AWWA standards is entirely voluntary. AWWA standards are intended to represent a consensus of the water supply industry that the product described will provide satisfactory service. When AWWA revises or withdraws this standard, an official notice of action will be placed on the first page of the classified advertising section of Journal AWWA. The action becomes effective on the first day of the month following the month of Journal AWWA publication of the official notice.

American National Standard An American National Standard implies a consensus of those substantially concerned with its scope and provisions. An American National Standard is intended as a guide to aid the manufacturer, the consumer, and the general public. The existence of an American National Standard does not in any respect preclude anyone, whether that person has approved the standard or not, from manufacturing, marketing, purchasing, or using products, processes, or procedures not conforming to the standard. American National Standards are subject to periodic review, and users are cautioned to obtain the latest editions. Producers of goods made in conformity with an American National Standard are encouraged to state on their own responsibility in advertising and promotional materials or on tags or labels that the goods are produced in conformity with particular American National Standards. CAUTION NOTICE: The American National Standards Institute (ANSI) approval date on the front cover of this standard indicates completion of the ANSI approval process. This American National Standard may be revised or withdrawn at any time. ANSI procedures require that action be taken to reaffirm, revise, or withdraw this standard no later than five years from the date of publication. Purchasers of American National Standards may receive current information on all standards by calling or writing the American National Standards Institute, 11 W. 42nd St., New York, NY 10036; (212) 642-4900.

All rights reserved. No part of this publication may be reproduced or transmitted in any form or by any means, electronic or mechanical, including photocopy, recording, or any information or retrieval system, except in the form of brief excerpts or quotations for review purposes, without the written permission of the publisher. Copyright © 1999 American Water Works Association Printed in USA

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Committee Personnel The AWWA Standards Committee on Polyelectrolytes, which reviewed and approved this standard, had the following personnel at the time of approval: Francis J. Mangravite, Chair Consumer Members T.A. Barber Jr., Coca-Cola Company, Portland, Ore. O.J. Dzydzora, United Water Services, Jersey City, N.J. D.W. Fredericksen, Erie County Water Authority, Lackawanna, N.Y. H.R. Hall,* City of Corpus Christi, Corpus Christi, Texas Sun Liang, Metropolitan Water District of Southern California, Los Angeles, Calif. S.R. Lohman, Denver Water Department, Denver, Colo. J.I. McKergow, Metro Toronto Works, Toronto, Ont. J.C. Routt, West Virginia-American Water Company, Charleston, W.V.

(AWWA) (AWWA) (AWWA) (AWWA) (AWWA) (AWWA) (AWWA) (AWWA)

General Interest Members P.E. Carlson, Safe Water Additives Institute, Pittsburgh, Pa. F.L. Hinker, Montgomery-Watson Engineers, Pasadena, Calif. W.D. Laraway, MPL Services Inc., Long Valley, N.J. D.R. Purkiss, NSF International, Ann Arbor, Mich. R.D. Letterman, Syracuse University, Syracuse, N.Y. F.J. Mangravite, Public Works Management Company, Morris Plains, N.J. J.H. Wilber,* Standards Engineer Liaison, AWWA, Denver, Colo.

(AWWA) (AWWA) (AWWA) (AWWA) (AWWA) (AWWA) (AWWA)

Producer Members F.W. Barvenik, CYTEC Industries, Stamford, Conn. S.R. Kurowsky, Callaway Chemical Company, Columbus, Ga. C.B. Lind, General Chemical Corporation, Syracuse, N.Y. C.C. Pintner, CPS Chemical Company, Memphis, Tenn. K.S. Salmen, Nalco Chemical Company, Naperville, Ill.

* Liaison, nonvoting

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Contents All AWWA standards follow the general format indicated subsequently. Some variations from this format may be found in a particular standard. SEC.

PAGE

SEC.

PAGE

Foreword

3

Definitions .......................................... 2

I I.A I.B I.C II II.A II.B III III.A

4 4.1 4.2 4.3 4.4 4.5 4.6

Requirements Description ............................................ Qualifications........................................ Chemical and Physical Requirements..................................... Impurities.............................................. Additives Requirements....................... Product Certifications ..........................

3 3 4 4

Standard

5 5.1 5.2 5.3 5.4 5.5

Verification General .................................................. Sampling ............................................... Visual Inspection .................................. Test Procedures .................................... Rejection................................................

4 4 5 5 8

1 1.1 1.2 1.3

General Scope ...................................................... 1 Purpose .................................................. 1 Application............................................. 1

6 6.1 6.2 6.3

Delivery Marking................................................. 8 Packaging and Shipping ...................... 9 Affidavit of Compliance........................ 9

2

References ........................................... 1

III.B IV V

Introduction........................................ vii Background......................................... vii History ................................................ vii Acceptance ......................................... viii Special Issues .................................... viii Safety ................................................. viii Spill Control ......................................... ix Use of This Standard........................... ix Development of a Purchase Specification ...................................... ix Modification to Standard..................... xi Major Revisions.................................... xi Comments............................................. xi

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Foreword This foreword is for information only and is not a part of ANSI/AWWA B452. I. Introduction. I.A. Background. Chemical clarification methods have been used to improve the quality of drinking water supplies since the late 1880s. In 1967, the first completely synthetic organic polyelectrolyte was accepted by the US Public Health Service for use in treating potable water. The responsibility for accepting additives for drinking water treatment was subsequently assumed by the US Environmental Protection Agency (USEPA) and administered by their Office of Drinking Water as an advisory program. The USEPA’s acceptance was made by the specific name of the suppliers’ product and not by generic type. Epichlorohydrin dimethylamine (EPI–DMA) polyamines (CAS* Nos. 25988-97-0 and 42751-79-1) are one of several types of synthetic organic polyelectrolytes that were accepted for use in potable water treatment under this program, which was discontinued in 1990. EPI–DMA polyamines are a family of synthetic organic polyelectrolytes (also called polymers or coagulants) used in water treatment to improve the performance of some unit operations in the treatment process, most often by increasing the extent or rate of liquid–solids separation. EPI–DMA polyamines are principally made from two monomers, epichlorohydrin (EPI) and dimethylamine (DMA). EPI–DMA polyamines have a cationic charge, a high relative charge density, and a low relative molecular weight. Because of this low molecular weight, they are manufactured and sold in solution form. The important concepts to remember regarding EPI–DMA polyamines include the following: 1. EPI–DMA polyamines are similar to polyDADMAC polymers (ANSI/AWWA B451) in their use, handling, storage, and solution preparation. 2. EPI–DMA polyamines are different from polyacrylamide (PAM) polymers (ANSI/AWWA B453) in their use, handling, storage, and solution preparation. 3. EPI–DMA polyamines are supplied in a solution form that may be referred to as liquids or aqueous solutions. 4. EPI–DMA polyamines are a family of polymers with a relatively constant charge type and charge density but with different molecular weights and degrees of branching. 5. The physical properties of EPI–DMA polyamines cannot usually be used to judge product performance. Only laboratory testing, pilot plant studies, or full plant trials can discern product efficacy. 6. EPI–DMA polyamines may contain inactive ingredients, such as salts, depending on the manufacturing method and formulation. The user should consult the material safety data sheet (MSDS) for product composition information regarding any specific EPI–DMA polyamine product. I.B. History. The AWWA Standards Council authorized development of this standard in 1979. The standard was developed by the AWWA Standards Committee on Polyelectrolytes and was approved by the AWWA Board of Directors on June 17, 1990. The second edition of this standard was approved on June 21, 1998.

*Chemical Abstracts Service, 2540 Olentangy River Rd., P.O. Box 3012, Columbus, OH 83210.

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I.C. Acceptance. In May 1985, the US Environmental Protection Agency (USEPA) entered into a cooperative agreement with a consortium led by NSF International (NSF) to develop voluntary third-party consensus standards and a certification program for all direct and indirect drinking water additives. Other members of the original consortium included the American Water Works Association Research Foundation (AWWARF) and the Conference of State Health and Environmental Managers (COSHEM). The American Water Works Association (AWWA) and the Association of State Drinking Water Administrators (ASDWA) joined later. In the United States, authority to regulate products for use in, or in contact with, drinking water rests with individual states.* Local agencies may choose to impose requirements more stringent than those required by the state. To evaluate the health effects of products and drinking water additives from such products, state and local agencies may use various references, including two standards developed under the direction of NSF, ANSI†/NSF‡ 60, Drinking Water Treatment Chemicals— Health Effects, and ANSI/NSF 61, Drinking Water System Components—Health Effects. Various certification organizations may be involved in certifying products in accordance with ANSI/NSF 60. Individual states or local agencies have authority to accept or accredit certification organizations within their jurisdiction. Accreditation of certification organizations may vary from jurisdiction to jurisdiction. Appendix A, “Toxicology Review and Evaluation Procedures,” to ANSI/NSF 60 (61) does not stipulate a maximum allowable level (MAL) of a contaminant for substances not regulated by a USEPA final maximum contaminant level (MCL). The MALs of an unspecified list of “unregulated contaminants” are based on toxicity testing guidelines (noncarcinogens) and risk characterization methodology (carcinogens). Use of Appendix A procedures may not always be identical, depending on the certifier. AWWA B452-98 addresses additives requirements in Sec. 4.5 of the standard. The transfer of contaminants from chemicals to processed water or to residual solids is becoming a problem of greater concern. The language in Sec. 4.5 is a recommendation only for direct additives used in the treatment of potable water to be certified by an accredited certification organization in accordance with ANSI/NSF Standard 60, Drinking Water Treatment Chemicals—Health Effects. However, users of this standard may opt to make this certification a requirement for the product. Users of this standard should consult the appropriate state or local agency having jurisdiction in order to 1. Determine additives requirements, including applicable standards. 2. Determine the status of certifications by all parties offering to certify products for contact with, or treatment of, drinking water. 3. Determine current information on product certification. II. Special Issues. II.A. Safety. EPI–DMA polyamines are not considered to be toxic as household products nor primary skin irritants by the Consumer Product Safety Commission

*Persons in Canada, Mexico, and non-North American countries should contact the appropriate authority having jurisdiction. †American National Standards Institute, 11 W. 42nd St., New York, NY 10036. ‡NSF International, 3475 Plymouth Rd., Ann Arbor, MI 48113-0140.

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(US Federal Hazardous Substances Act). Good housekeeping procedures and personal cleanliness are recommended when handling EPI–DMA polyamines. Safety glasses should be worn when handling EPI–DMA polyamines. Good first-aid practices should be followed in all cases of exposure. In case of eye contact, flush with plenty of water for at least 15 min. If irritation develops, call a physician. Consult the material safety data sheet (MSDS) for the specific product for safety procedures before handling any EPI–DMA polyamines. II.B. Spill Control. EPI–DMA polyamines should be disposed of according to local, state or provincial, and federal regulations. A dike should be formed around the spill area to contain as much material as possible. Any remaining material should be removed by adsorbing it on vermiculite or other suitable adsorbing material and placed in a sealable metal container for disposal. The spill area should be thoroughly hosed with water after all possible polymer has been scooped up, absorbed, or wiped up because liquid product can make floors very slippery. Use of warm water is beneficial. III. Use of This Standard. AWWA has no responsibility for the suitability or compatibility of the provisions of this standard to any intended application by any user. Accordingly, each user of this standard is responsible for determining that the standard’s provisions are suitable for and compatible with that user’s intended application. III.A. Development of a Purchase Specification. This AWWA standard can be used to prepare a purchase specification, but is not itself a specification because it cannot address requirements unique to the purchaser’s specific situation and does not establish business relationships. In addition, this EPI–DMA polyamines standard does not establish physical and chemical property specifications for any one EPI– DMA polyamine product, because the physical and chemical properties of EPI–DMA polyamines do not always relate to their performance as a coagulant in specific applications. Following in Sec. III.A.1 through III.A.5 are requirements that the user may consider to develop an EPI–DMA polyamines product purchase specification: III.A.1 General Product Requirements (for multiple products). The following items should be covered in the purchaser’s specifications. 1. Standard used—that is, ANSI/AWWA B452, Standard for EPI–DMA Polyamines, of latest revision. 2. Whether the recommended compliance with ANSI/NSF Standard 60, Drinking Water Treatment Chemicals—Health Effects is to be required. If this certification is to be required, the purchaser specifications shall read, “This material shall be certified as suitable for treatment of drinking water by an accredited certification program in accordance with ANSI/NSF Standard 60, Drinking Water Treatment Chemicals—Health Effects.” 3. Compliance with USEPA Phase II Rule National Primary Drinking Water Regulations, epichlorohydrin treatment technique requirements (40 CFR 141.111). 4. Approval by or certification as meeting any applicable state, provincial, or local requirements. 5. The EPI–DMA polyamines supplied according to this standard shall contain no substances in quantities capable of producing deleterious or injurious effects on those consuming water that has been treated with EPI–DMA polyamines in accordance with the supplier’s recommendations and within the maximum allowed dosage.

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Upon request, the supplier shall provide an estimate of the impurities. This estimate shall be based on the maximum concentration of residual monomer (dimethylamine, epichlorohydrin) or impurity present and shall be reported as less than or equal to the maximum concentration. NOTE: It may not be possible for the supplier to routinely provide the precise value of the residual impurities of each EPI–DMA polyamines shipment. Such measurements are conducted on each manufactured batch, which may then be continuously added to bulk storage tanks from which shipments are continuously extracted. III.A.2 User-Specific Requirements. 1. Description of application. 2. Estimated annual purchase requirements lb (kg). 3. Typical order quantity lb (kg). 4. Packaging (pails, drum and drum size, drum types, returnable semibulk containers, nonreturnable semibulk containers, bulk by truck, bulk by rail). 5. Sampling requirements (Sec. 5.2). 6. Marking requirements (Sec. 6.1). 7. Shipping requirements (Sec. 6.2). 8. Delivery requirements (need for: truck with a lift gate; length and coupling sizes of hose needed for bulk delivery; transfer pump; allowed times of delivery; limitations on truck size or weight; sampling protocol; other). 9. Order lead time (number of working days between order placement and delivery necessary if typical lead times are not sufficient). 10. Affidavit of Compliance (Sec. 6.3). 11. Origin of material (Sec. 5.8.1). 12. Shipping and billing addresses. 13. Financial terms. 14. Insurance/performance bond requirements. 15. Physical property limitations: If the purchaser knows that certain physical properties cannot be handled by the storage or feed equipment, these properties should be stated. 16. Other user-specific requirements. III.A.3 Polymer Content. If the purchaser does not know which type of EPI– DMA polyamine is required, the purchaser need not specify the polymer content. Once a specific product and supplier are chosen, the supplier should be required to provide the percent by weight of polymer in the product. III.A.4 Specific Physical and Chemical Product Properties (Quality Control). Minimum specifications for determining specific product properties should include visual inspection, total solids, and Brookfield viscosity. 1. Visual inspection (Sec. 4.3.1, 5.3). A quick, useful qualitative test for all EPI–DMA polyamines products. 2. Total solids (Sec. 4.3.2, 5.4.1). Should be used as a specification as it relates to active polymer content and is important information needed to interpret other tests. 3. Brookfield viscosity (Sec. 4.3.3, 4.3.4, 5.4.2, 5.4.3). Many suppliers provide for each product the Brookfield viscosity ranges of both a specific concentration of the product and the bulk (undiluted) product. The product concentration and specific Brookfield viscosity test procedure used by the supplier should be used whenever possible. Once a specific EPI–DMA polyamine product has been chosen, the measurement of bulk Brookfield viscosity is a valuable way to determine if there may be a product quality variation. If multiple EPI–DMA polyamine products are being

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evaluated, the measurement of Brookfield viscosity of a specific polymer solution concentration can be a helpful means of comparison. 4. pH of a solution (Sec. 5.4.4). The pH of EPI–DMA polyamines might be helpful in confirming a quality problem but the pH itself does not directly relate to polymer performance. Many suppliers provide the pH range of a specific concentration of each product. III.A.5 Product Performance. Performance evaluation via a laboratory jar test or other performance test is essential for confirming EPI–DMA polyamine activity. It is the only way to consider possible changes in the water composition, temperature, or in the type or amount of other chemicals added along with the EPI–DMA polyamines. III.B. Modification to Standard. Any modification of the provisions, definitions, or terminology in this standard must be provided in the purchaser’s specifications. IV. Major Revisions. Major changes made to the standard in this revision include the following: 1. The format has been changed to AWWA standard style. 2. The acceptance clause (Sec. I.C) and requirements (Sec. 4.4.3 and 5) have been revised to approved wording and the consideration of multiple applications. 3. The foreword has been expanded to include development of a purchase specification. 4. The analytical procedure for analyzing residual epichlorohydrin and other chlorine-containing residuals has been standardized with ANSI/NSF 60. V. Comments. If you have any comments or questions about this standard, please call the AWWA Volunteer and Technical Support Group, (303) 794-7711 ext. 6283, FAX (303) 794-1440, or write to the department at 6666 W. Quincy Ave., Denver, CO 80235.

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American Water Works Association R

ANSI/AWWA B452-98 (Revision of ANSI/AWWA B452-90)

AWWA STANDARD FOR

EPI–DMA POLYAMINES SECTION 1: GENERAL Sec. 1.1

Scope This standard covers epichlorohydrin dimethylamine (EPI–DMA) polyamines for water supply service applications.

Sec. 1.2

Purpose The purpose of this standard is to provide the minimum general requirements for EPI–DMA polyamine products, including physical, chemical, packaging, shipping, and testing requirements and to provide the means of developing requirements for specific EPI–DMA polyamine products.

Sec. 1.3

Application This standard can be referenced in specifications for purchasing and receiving EPI–DMA polyamine products, and can be used as a guide for testing the physical and chemical properties of EPI–DMA polyamine product samples. The stipulations of this standard apply when this document has been referenced and then only to EPI– DMA polyamines used in water supply service applications.

SECTION 2: REFERENCES This standard references the following documents. In their latest editions, they form a part of this standard to the extent specified within the standard. In any case of conflict, the requirements of this standard shall prevail. ANSI*/AWWA B451—Standard for Poly(Diallydimethylammonium Chloride). ANSI/AWWA B453—Standard for Polyacrylamide.

*American National Standards Institute, 11 W. 42nd St., New York, NY 10036.

1 Copyright © 1999 American Water Works Association, All Rights Reserved.

2 AWWA B452-98

Standard Methods for the Examination of Water and Wastewater. APHA,* AWWA, WEF.† Denver, Colo. (19th edition, 1995). Code of Federal Regulations, Title 40, CFR, Parts 141.111.‡ USEPA Phase II Rule National Primary Drinking Water Regulations, epichlorohydrin treatment technique requirements. ANSI/NSF§ Standard 60, Drinking Water Treatment Chemicals—Health Effects.

SECTION 3: DEFINITIONS The following definitions shall apply in this standard: 1. Manufacturer: The party that manufactures, fabricates, or produces materials or products. 2. Purchaser: The person, company, or organization that purchases any materials, products, or services to be performed. 3. Supplier: The party that supplies materials, products, or services. A supplier may or may not be the manufacturer. 4. Polymer: The EPI–DMA polyamine polymer in the product, also called active polymer. 5. Product: The commercial material “as sold” containing polymer. May contain other substances such as water.

SECTION 4: REQUIREMENTS Sec. 4.1

Description EPI–DMA polyamines are polyquaternary polymers produced from the reaction of dimethylamine and epichlorohydrin. Products that contain the EPI–DMA polyamines may also contain residual amounts of epichlorohydrin and dimethylamine as well as byproducts of chemical transformation of epichlorohydrin, including 1,3-dichloro-2-propanol and 2,3-dichloro-1-propanol or impurities of raw materials that may carry through the manufacturing process. EPI–DMA polyamines are sold as aqueous solutions in a wide range of molecular-weights. The higher relative molecular weights are obtained by adding small amounts of branching agents such as ammonia or ethylenediamine.

Sec. 4.2

Qualifications Because EPI–DMA polyamines are a family of polymers, qualifications for the physical and chemical requirements described in Sec. 4.3 and 4.4 cannot be generically set. More importantly, none of the physical or chemical requirements in

*American Public Health Association, 1015 15th St. N.W., Washington, DC 20005. †Water Environment Federation, 601 Wythe St., Alexandria, VA 22314-1994. ‡Superintendent of Documents, US Government Printing Office, Washington, DC 20402. §NSF International, 3475 Plymouth Road, P.O. Box 130140, Ann Arbor, MI 48113-0140.

Copyright © 1999 American Water Works Association, All Rights Reserved.

EPI–DMA POLYAMINES

3

this standard can be used to identify the EPI–DMA polyamine product with the best performance in a specific application. Only actual performance testing can determine this. Therefore, these requirements are best used to ensure product quality and uniformity after a specific EPI–DMA polyamine product has been chosen for use. The purchaser should set the specifications for each specific EPI–DMA polyamine product individually. This is best done in cooperation with the supplier and/or manufacturer employing the manufacturer’s own quality control specifications or, if the former is not available, the stated ranges of properties from the specific product’s product data (information or fact) sheet and material safety data sheet (MSDS). The purchaser may want to limit the specification to those properties that are most meaningful (Sec. III of the foreword).

Sec. 4.3

Chemical and Physical Requirements The chemical and physical requirements shall be determined by the methods specified in Sec. 5, Verification, or other methods acceptable to both the purchaser and supplier. 4.3.1 Appearance (visual inspection). The clear-colored EPI–DMA polyamine product shall be free from visible foreign matter and sediment. Color may vary from colorless to amber. Color has no known effect on product performance. Viscosity may vary from relatively low to relatively high depending on the individual product’s polymer content and molecular weight (Sec. 5.3). 4.3.2 Total solids. EPI–DMA polyamines are sold as aqueous solutions. Individual products vary in polymer content and total solids from less than 10 percent to greater than 65 percent by weight (Sec. 5.4.1). The total solids of an EPI–DMA polyamine product may be the same as or greater than the polymer content. Stated differently, the polymer content of a product cannot be greater than its total solids. The possible presence of inert or inactive ingredients is the reason total solids and polymer content may be different. The supplier should be willing to reveal the polymer (active polymer) content of a specific product. The difference between the measured total solids and the supplier’s stated active polymer content is the nonvolatile inert and/or inactive solids of the product. Requirements vary with each product (Sec. 5.4.1). 4.3.3 Bulk Brookfield viscosity. The bulk Brookfield viscosity (viscosity of the liquid EPI–DMA polyamine product as sold) requirements vary with each product. Over the entire family of products, product bulk viscosities typically range from, but are not limited to (not a specification), 70 to 8,000 centipoise (Sec 5.4.2). 4.3.4 Brookfield viscosity of a specific solution concentration. Requirements vary with each product (Sec. 5.4.3). 4.3.5 pH of a solution. Requirements vary with each product (Sec. 5.4.4).

Sec. 4.4

Impurities 4.4.1 General. EPI–DMA polyamines supplied according to this standard shall contain no substances in quantities capable of producing deleterious or injurious effects to the health of those consuming water that has been treated with EPI–DMA polyamines in accordance with the supplier’s recommendations and within the maximum allowed dosage. 4.4.2 Specific. The following requirements shall apply to each EPI–DMA polyamine product: 1. Epichlorohydrin levels shall not exceed 20 mg/kg on a polymer basis.

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4 AWWA B452-98

2. Total chlorine-containing residuals shall not exceed a level of 2,000 mg/kg on a polymer basis. 3. No individual chlorine-containing species of residual shall exceed a level of 1,000 mg/kg on a polymer basis. EPI–DMA polyamines may contain measurable amounts of inorganic salts, such as sodium chloride.

Sec. 4.5

Additives Requirements The user of EPI–DMA polyamines shall comply with the following additive requirements: 1. Maximum use level specified for each specific EPI–DMA polyamine product by the agency certifying the product under ANSI/NSF Standard 60, Drinking Water Treatment Chemicals—Health Effects. 2. Maximum use levels established by the USEPA Phase II Rule National Primary Drinking Water Regulations, epichlorohydrin treatment technique requirements. 3. Any state, provincial, or local requirements including approval, certification, and additive requirements. 4. The user of EPI–DMA polyamines should be aware of the possibility that there may be more than one application of EPI–DMA polyamines in their water supply system and that the additive requirements should apply to the aggregate maximum effective use level of all applications.

Sec. 4.6

Product Certifications EPI–DMA polyamines are direct additives used in the treatment of potable water. These materials should be certified as suitable for contact with or treatment of drinking water by an accredited certification organization in accordance with ANSI/ NSF Standard 60, Drinking Water Treatment Chemicals—Health Effects. Evaluation shall be accomplished in accordance with requirements that are no less restrictive than those listed in ANSI/NSF Standard 60. Certification shall be accomplished by a certification organization accredited by the American National Standards Institute.

SECTION 5: VERIFICATION Sec. 5.1

General The methods provided in this standard are acceptable for determining variations in EPI–DMA polyamine product physical and chemical properties, but may not provide exactly the same quantitative result as another method of equally sound basis.

Sec. 5.2

Sampling All sampling should be done at the point of destination. Each sample shall be sealed in a dry, airtight plastic or glass container and carefully identified with a label to include the following information: date and place of the sampling, product name/ number, lot number, name of supplier, and name of sampler. Three samples of each lot or shipment should be taken for compliance with the rejection procedure (Sec. 5.5). Samples shall be taken from each tank car, tank truck, returnable or nonreturnable bin, or a representative drum or pail. Samples should be thoroughly

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EPI–DMA POLYAMINES

5

shaken before each test portion analyzed. Laboratory examination of the sample should be completed as soon as possible. Sample size should be at least 8 oz (200 mL). NOTE: Samples should be disposed of as soon as possible after they reach their stated shelf life.

Sec. 5.3

Visual Inspection Visual inspection is the easiest qualitative test that can be used for quality assurance of EPI–DMA polyamine products. It is essential that the sample being inspected is taken properly, stored properly, and inspected as soon as possible during or after the shipment of product is received. The sample shall be observed individually and may also be compared to a previously acceptable sample that has been stored properly and is within its shelf life.

Sec. 5.4

Test Procedures 5.4.1 Total solids. This procedure is one of several that are applicable to determining the total solids content of EPI–DMA polyamine products. The procedure is not corrected for inert ingredients, therefore, it may not give the polymer content of the sample. 5.4.1.1 Apparatus. 1. Analytical balance. 2. Aluminum weighing dish. 3. Dropper pipettes or syringes, glass or plastic, 1.0 to 10 mL. 4. Forced draft oven, capable of maintaining temperature at ±2°C of set point. 5. Desiccator and desiccant. 5.4.1.2 Procedure. 1. Heat aluminum pans in oven at 105°C for a minimum of 1 h; remove and cool in a desiccator. 2. Record tare weight of aluminum weighing pan to nearest 0.0001 g. 3. Using a syringe or dropper pipette, dispense sufficient EPI–DMA polyamine product in the weighing dish to yield a desired residue of 0.45 g ±0.05 g. Record the total weight of the sample plus the weighing dish to the nearest 0.0001 g. For a typical EPI–DMA polyamine product, add 0.9 g to 4.5 g, depending on the product. Spread the sample over the surface of the aluminum dish to avoid formation of a crust during drying. It may be necessary to add 3 to 5 mL of deionized water to assist spreading. 4. Place the aluminum weighing dish containing the weighed sample in a 105° to 110°C forced draft oven for 3 h. 5. Remove aluminum dish from the oven and cool in a desiccator. Weigh the cooled dish to the nearest 0.0001 g. 5.4.1.3 Calculation. % total solids =

(Eq 1)

( weight of dish + dry sample ) – ( weight of empty dish ) ------------------------------------------------------------------------------------------------------------------------------------------------------ × 100 ( weight of dish + wet sample ) – ( weight of empty dish ) 5.4.1.4 Notes. 1. Samples should be run in duplicate. 2. The difference between duplicate samples should be less than ±0.5 percent. If it is greater than ±0.5 percent, the test should be rerun.

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6 AWWA B452-98

5.4.2 Bulk Brookfield viscosity. A Brookfield Synchro-Lectric LVT viscometer* or equivalent is used. The readings are taken with an appropriate spindle number at an appropriate spindle speed, at a constant temperature. The spindle number needed depends on viscosity range of the specific product being analyzed. The viscosity of EPI–DMA polyamine solutions increases with polymer/solids and molecular weight. EPI–DMA polyamine solutions are thixotropic such that their viscosity will decrease with increasing spindle speed. It is best to use the spindle and speed used by the manufacturer of the product for quality control purposes. However, in the absence of such information, a speed of 12 rpm may be used and the spindle varied to give a reading in the center of the viscometer’s range. 5.4.2.1 Apparatus. 1. Viscometer, Brookfield, Model LVT or equivalent. 2. Beaker, 180-mL tall form Griffin or other container of equal diameter and depth. 5.4.2.2 Procedure. 1. Set up the viscometer without the guard attached. Level the instrument. 2. Attach the spindle specified by the polymer supplier. (NOTE: Left-handed threads.) If no specific spindle is specified by the manufacturer, start with spindle No. 1 and proceed through step 9, and then repeat steps 2 through 9, if necessary, with increasing spindle numbers, until a spindle is found that gives a reading in step 9 that is in the middle of the viscometer’s scale range. 3. Pour enough sample into the container to cover the spindle up to the groove. 4. Adjust the temperature of the sample to 25.0°C±1.0°C. 5. Lower the viscometer with the spindle attached into the sample until the surface of the sample is at the groove on the spindle shaft. The spindle should not contact the bottom of the container. 6. Set the viscometer to the chosen rpm. 7. Turn on the viscometer motor. 8. After the needle reaches a steady reading and after at least 10 revolutions, depress the clutch lever on the back of the viscometer to “freeze” the needle on the scale. With the clutch depressed, stop the viscometer motor when the needle is visible in the viscometer window. 9. Read and record the position of the needle on the scale. 10. Repeat steps 7 to 9 to obtain three readings. 5.4.2.3 Calculations. 1. Average the three readings. 2. Obtain the Brookfield viscosity by multiplying the average reading calculated in step 1 by the factor for that spindle and speed supplied by the viscometer manufacturer. 5.4.3 Brookfield viscosity of an EPI–DMA polyamine solution. Choose a concentration and the basis of the concentration (weight or volume) to be prepared. Prepare the solution. Measure the Brookfield viscosity by the method described in Sec. 5.4.2. Preferably, the concentration and basis of concentration should be chosen from the supplier’s product data sheet specification or supplier’s actual product quality control procedure.

*Brookfield Engineering Laboratories Inc., Stoughton, Mass.

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EPI–DMA POLYAMINES

7

5.4.4 pH of a solution. 5.4.4.1 Apparatus. 1. pH meter. 2. Fiber junction and reference electrode. 3. pH reference buffer solutions. 4. 180-mL tall form Griffin beaker or equivalent. 5. Thermometer. 6. EPI–DMA polyamine product solution. The specific concentration of the solution should be chosen from the supplier’s product literature. Alternatively, the solutions prepared for either the Brookfield viscosity of an EPI–DMA polyamine solution test (Sec. 5.4.3) can be used. 5.4.4.2 Procedure. 1. Standardize the pH meter with buffer solutions above and below the pH range to be tested. 2. Add polymer solution to a 180-mL beaker. 3. Adjust the temperature setting of the pH meter to that of the polymer solution, which should be at room temperature, 25°C±2°C. 4. Measure the pH of the polymer solution. 5. Thoroughly rinse the electrodes after each test. 5.4.5 Percent sodium chloride. 5.4.5.1 Procedure. Determine sodium content by atomic absorption spectrophotometry or sodium ion electrode analysis using standard techniques as described in the latest edition of Standard Methods for the Examination of Water and Wastewater. 5.4.5.2 Calculation. Calculate NaCl content: 58.5 % NaCl = % Na × ----------23 5.4.6 Other inorganic impurities. Inorganic impurities other than sodium chloride, if any, shall be determined by the procedures described in the latest edition of Standard Methods for the Examination of Water and Wastewater or by other accepted, applicable techniques. 5.4.7 Determination of EPI–DMA polyamine. This procedure is one of several that are applicable to the determination of EPI–DMA polyamine. This particular procedure determines the total solids in the sample and the NaCl content. The polymer content is then calculated as follows: % EPI–DMA polyamine = % total solids – % NaCl Total solids are determined by the procedure in Sec. 5.4.1 and NaCl from the procedure in Sec. 5.5.1. The previous equation assumes that sodium chloride is the only inorganic salt present. 5.4.8 Determination and quantification of residual epichlorohydrin, 1,3-dichloro2-propanol and 2,3-dichloro-1-propanol, and in EPI–DMA polyamine. In this procedure, the epichlorohydrin (EPI), 1,3-dichloro-2-propanol (DCIPA) and 2,3-dichloro1-propanol (DCP) are extracted from the polymer with a 50/50 (v/v) solution of isopropanol/chloroform, followed by chromatographic separation, and quantified by using gas chromatography (GC) with flame ionization detection. The analytical procedure used should be that described in the ANSI/NSF Standard 60.

Copyright © 1999 American Water Works Association, All Rights Reserved.

8 AWWA B452-98

ANSI/NSF Standard 60—1997 edition describes this analytical procedure in Appendix B.

Sec. 5.5

Rejection* A written statement explaining the nature of dissatisfaction with the shipment of EPI–DMA polyamine based on this standard must be received by the manufacturer or supplier within 30 working days after the receipt of the shipment at the point of destination. If the manufacturer or supplier desires a retest, they shall notify the purchaser within five working days of receipt of the complaint. On receipt of the request for a retest, the purchaser shall forward the manufacturer or supplier one of the sealed samples per Sec. 5.2. In the event that the results obtained by the manufacturer’s or supplier’s retest do not agree with the results obtained by the purchaser, the third sealed sample shall be forwarded, unopened, for analysis to a referee laboratory agreed on by both parties. The results of the referee analysis shall be accepted as final. 5.5.1 Material origin outside of North America. At the request of the purchaser, the supplier shall inform the purchaser of the origin of the material to be furnished. If the material furnished according to this standard was manufactured outside of the country of use, the supplier assumes full and complete responsibility for the product’s compliance with this standard. The purchaser may request that the supplier put in writing the steps to be taken to ensure that the material supplied conforms to the standard.

SECTION 6: DELIVERY† Sec. 6.1

Marking 6.1.1 Required. Each shipment of EPI–DMA polyamine shall carry with it some means of identification. The net weight of the contents, the name of the supplier, the country of origin, the brand name, if any, the product number, and the lot number shall be legibly marked on each package. 6.1.2 Optional. Packages may also bear the statement, “Guaranteed by (name of supplier or manufacturer) to meet the AWWA Standard for EPI–DMA Polyamine,” provided that the requirements of this standard are met and the material is not of a different quality based on a separate agreement between the supplier and purchaser.

*There is an associated uncertainty or lack of precision involved with the experimental determination of any value. Therefore, when comparing measured values with those indicated by the manufacturer’s or supplier’s affidavit of compliance, the value indicated by the affidavit of compliance should fall within the range of the measured value, that is, within the range set by the average and its standard deviation. †Governmental packaging and marking references reflect US requirements. Users of EPI–DMA polyamines in Canada, Mexico, and non-North American countries should verify applicable local and national regulatory requirements.

Copyright © 1999 American Water Works Association, All Rights Reserved.

EPI–DMA POLYAMINES

Sec. 6.2

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Packaging and Shipping EPI–DMA polyamines are supplied in drums, returnable or non-returnable bins, pails, or in bulk. If shipped in bulk by tank car, tank truck, or railcar, the tanks shall be thoroughly cleaned before shipping EPI–DMA polyamine. All truck shipments shall be accompanied by weight tickets, which are machine printed and dated. The shipper shall follow all local, state or provincial, federal, and US Department of Transportation (USDOT) requirements.*

Sec. 6.3

Affidavit of Compliance The purchaser may require the manufacturer or supplier to furnish an affidavit attesting that the EPI–DMA polyamine product furnished under the purchaser’s specifications complies with all applicable requirements of this standard.

* Because of frequent changes in regulations, the purchaser’s specifications should not attempt to describe the actual regulations.

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