Ammonium Sulfate

Effective date: June 1, 2023.

First edition approved by Board of Directors July 15, 1949.
This edition approved Jan. 12, 2023.
Approved by American National Standards Institute Jan. 31, 2023.

�\ STANDARD

American Water Works

Association
'\\.I Since 1881
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. This standard does not supersede or take precedence over or displace any
applicable law, regulation, or code of any governmental authority. AWWA standards are intended to represent a consensus
of the water industry that the product described will provide satisfactory service. When AWWA revises or withdraws this
standard, an official notice of action will be placed in the Official Notice 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
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conformity with particular American National Standards.

CAUTION NoT1cE: 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 This American National Standard may be revised or withdrawn at any time.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 ANSI approval. Purchasers of American National Standards may receive current information on all standards
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All rights reserved. No part of this publication may be

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ISBN-13, print: 978-1-64717-132-2 ISBN-13, electronic: 978-1-61300-663-4

DOI: http://dx.doi.org/10.12999/AWWA.8302.23

All rights reserved. No part of this publication may be reproduced or transmitted in any form or by any means,
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commercial use of this material is prohibited, except with written permission from the publisher.

Copyright© 2023 by American Water Works Association

Printed in USA

ii
 Committee Personnel

The AWWA Standards Committee on Disinfectants, which developed and approved this standard,
had the following personnel at the time of approval:

K. Blake Stark, Chair

General Interest Members

S.M. Alpert (liaison, nonvoting), Standards Council Liaison, Hazen and Sawyer, Nashville, Tenn.
K-K Au, Consultant, Naperville, Ill.
N.J. Edman (liaison, nonvoting), Standards Group Liaison, AW WA, Denver, Colo.
M.C. Graves, Weston Solutions Inc., Austin, Tex.
R. Hampaul, Indigenous Services Canada, Nanaimo, B.C.
K.B. Stark, NSF International, Ann Arbor, Mich.
A. Waldron, City of Englewood, Englewood, Colo.

Producer Members
E.M. Meyer, Solenis, Charleston, Tenn.
J. Mock, Olin Corporation, Cleveland, Tenn.
D. Stein, The Chlorine Institute, Arlington, Va.
D.S. Weatherup, De Nora Water Technologies, Colmar, Pa.

User Members
R.C. Lorenz, Westerville Water Plant, Westerville, Ohio
F. Noce, Lake County Department of Utilities, Painesville, Ohio

L. Olson, New Jersey American Water, Colts Neck, N.J.

P.R. Riendeau, New England Water Works Association, Holliston, Mass.

iii
This page intentionally blank.
 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 2 References ...................................... 2

I Introduction .................................... vu 3 Definitions ..................................... 2

I.A Background ..................................... vii
4 Requirements
LB History ............................................ vu
4.1 Physical Requirements ..................... 3
LC Acceptance ...................................... Vlll
4.2 Chemical Requirements .................. 3
II Special Issues ................................... IX

III Use of This Standard ....................... IX

4.3 Impurities........................................ 3

III.A Purchaser Options and Alternatives ... ix 5 Verification

III.B Modification to Standard ................ x 5.1 Sampling ......................................... 4

IV Major Revisions............................... x
5.2 Test Procedures................................ 5
v Comments ...................................... x
5.3 Notice of Nonconformance ............. 10

Standard 6 Delivery

1 General 6.1 Marking .......................................... 11

1.1 Scope............................................... 1 6.2 Packaging and Shipping .................. 11
1.2 Purpose ........................................... 1
6.3 Affidavit of Compliance or Certified
1.3 Application...................................... 1 Analysis ..................................... 12

v
This page intentionally blank.
 Foreword
This foreword is for information only and is not a part of ANSI*/AWWA B302.

I. Introduction.

I.A. Background. Ammonium sulfate, (NH4hS04, is used by some water

utilities as a source of ammonia in the formation of chloramines and as an activating
agent in the formation of activated silica. It is readily soluble in water and consists
of rhombic crystals or fine granules that, if pure, are colorless or white and odorless.
Commercial grades of ammonium sulfate have a pinkish to brown color as a result of
traces of iron and organic compounds contained in the source of the material.
Ammonium sulfate used for potable water treatment is usually a byproduct in the
manufacture of caprolactam, a nylon-based material. It is available at a commercial
strength of 99 percent ammonium sulfate. Ammonium sulfate obtained as a byproduct
in the manufacture of coal gas and coke is no longer used in potable water treatment.
Ammonium sulfate can be prepared free of contaminants by reacting ammonia and
sulfuric acid. Food-grade ammonium sulfate, which is used as a dough conditioner and
in yeast food, is produced in this manner. The cost of the food-grade material is several
times greater than the commercial-grade material; however, some states require food­
grade material for use in potable water treatment.
Depending on its source, ammonium sulfate material has a tendency to cake and
arch when stored in bulk. This behavior can be prevented by the addition of a small
amount of amorphous silica (0.06-0.1 percent), a type of fused silica.
For safety precautions, refer to material safety data sheets (SDSs) available from the
supplier or manufacturer.
l.B. History The first edition of this standard was prepared by the AW WA
Water Purification Division. It was approved as tentative on July 15, 1949, and made
standard on May 15, 1953, with the designation of AWWA B400-53. The second
edition was prepared by AWWA Committee 7400P and was approved on Jan. 27,
1964, with the designation of AW WA B302-64. The third and fourth editions were
prepared by the AW WA Standards Committee on Taste and Odor Control Chemicals
and were approved on Jan. 25, 1981, and June 22, 1986, respectively. Subsequent
editions were prepared by the AWWA Standards Committee on Disinfectants and

* American National Standards Institute, 25 West 43rd Street, Fourth Floor, New York, NY 10036.

vii
approved by the Board of Directors on June 17, 1995; June 11, 2000; Jan. 16, 2005;
June 20, 2010; and June 19, 2016. This edition was approved on Jan. 12, 2023.
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 direct and indirect drinking water additives. Other members of
the original consortium included the Water Research Foundation (formerly AwwaRF)
and the Conference of State Health and Environmental Managers (COSHEM).
AW WA 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. t 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 four standards developed under the
direction of NSF*: NSF/ANSI/CAN§ 60, Drinking Water Treatment Chemicals­
Health Effects, NSF/ANSI/CAN 61, Drinking Water System Components-Health
Effects, NSF/ANSI/CAN 372, Drinking Water System Components-Lead Content,
and NSF/ANSI/CAN 600, Health Effects Evaluation and Criteria for Chemicals in
Drinking Water.
Various certification organizations may be involved in certifying products in
accordance with NSF/ANSI/CAN GO. Individual states or local agencies have authority
to accept or accredit certification organizations within their jurisdictions. Accreditation
of certification organizations may vary from jurisdiction to jurisdiction.
NSF/ANSI/CAN 600 (which formerly appeared in NSF/ANSI/CAN 60 and 61
as Annex A, "Toxicology Review and Evaluation Procedures") 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 NSF/ANSI/CAN 600
procedures may not always be identical, depending on the certifier.
ANSI/AW WA B302 addresses additives requirements in Sec. 4.3.4 of the standard.
The transfer of contaminants from chemicals to processed water or to residual solids is

t Persons outside the United States should contact the appropriate authority having jurisdiction.
* NSF International, 789 North Dixboro Road, Ann Arbor, MI 48105.
§ Standards Council of Canada, 55 Metcalfe Street, Suite 600, Ottawa, ON KIP 6L5 Canada

viii
becoming a problem of greater concern. The language in Sec. 4.3.4 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 NSF/ANSI/CAN 60, Drinking
Water Treatment Chemicals-Health Effects. However, users of the standard may opt
to make this certification a requirement for the product. Users of this standard should
also 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 parties offering to certify products
for contact with, or treatment of, drinking water.
3. Determine current information on product certification.

II. Special Issues. This standard has no applicable information for this
section.

III. Use of This Standard. It is the responsibility of the user of an AWWA

standard to determine that the products described in that standard are suitable for use
in the particular application being considered.
III.A. Purchaser Options and Alternatives. The following information should be
provided by the purchaser:
1. Standard used-that is, ANSI/AWWA B302, Ammonium Sulfate, of latest
revision.
2. Quantity of ammonium sulfate required.
3. Whether compliance with NSF/ANSI/CAN 60, Drinking Water Treatment
Chemicals-Health Effects, is required.
4. Details of federal, state, provincial, territorial, and local requirements
(Section 4).
5. Whether the ammonmm sulfate shall contain an anticaking agent
(Sec. 4.1.2).
6. Whether optional markings will be required (Sec. 6.1.2).
7. Method of packaging and shipping required (Sec. 6.2).
8. An affidavit of compliance or certified analysis, or both, if required
(Sec. 6.3).
9. Whether the purchaser will reject product from containers or packaging
with missing or damaged seals. The purchaser may reject product from bulk containers
or packages with missing or damaged seals unless the purchaser's tests of representative
samples, conducted in accordance with Sec. 5.2, demonstrate that the product meets
the standard. Failure to meet the standard or the absence of, or irregularities in, seals
may be sufficient cause to reject a shipment.

ix
 10. Whether alternative security measures have been adopted to replace or
augment the security measures set out in Sec. 6.2.3 and Sec. 6.2.4.
III.B. Modification to Standard. Any modification of the provisions, definitions,
or terminology in this standard must be provided by the purchaser.

IY. Major Revisions. Major changes made to the standard in this revision
include the following:
1. Minor boilerplate language updates in the following sections:
• I.C. Acceptance
• III.A. Purchaser Options and Alternatives
• Section 2: References
• Section 4: Requirements
• Sec. 4.3.4 Product Certifications
• Sec. 6.2.4.2 Chain of Custody

V. Comments. If you have any comments or questions about this standard,

please call AWWA Engineering and Technical Services at 303.794.7711; FAX at
303.795.7603; write to the department at 6666 West Quincy Avenue, Denver, CO
80235-3098; or email at standards@awwa.org.

x
 ANSl/AWWA8302-23
(Revision of ANSl/AWWA 8302-16)

American Water Works

Association
Dedicated to the World's Most Important Resource®
AWWA Standard

..
� ...... ______
.. _________

Ammonium Sulfate

SECTION 1: GENERAL

Sec. 1.1 Scope

This standard describes ammonium sulfate, (NH4hS04, for use m the
treatment of potable water, wastewater, and reclaimed water.

Sec. 1.2 Purpose

The purpose of this standard is to provide the minimum requirements for
ammonium sulfate, including physical, chemical, sampling, packaging, shipping,
and testing requirements.

Sec. 1.3 Application

This standard can be referenced in documents for purchasing and receiving
ammonium sulfate and can be used as a guide for testing the physical and chemical
properties of ammonium sulfate samples. The stipulations of this standard apply
when this document has been referenced and then only to ammonium sulfate used
in the treatment of potable water, wastewater, and reclaimed water.
2 AWWA 8302-23

SECTION 2: REFERENCES

This standard references the following document. In its latest edition, it forms
a part of this standard to the extent specified within the standard. In any case of
conflict, the requirements of this standard shall prevail.
NSF*/ANSit/CAN:J: 60-Drinking Water Treatment Chemicals-Health
Effects.

SECTION 3: DEFINITIONS

The following definitions shall apply in this standard:

1. Day: A 24-h period.
2. Manufacturer: The party that manufactures, fabricates, or produces
materials or products.
3. Potable water: Water that is safe and satisfactory for drinking and
cooking.
4. Purchaser: The person, company, or organization that purchases any
materials or work to be performed.
5. Reclaimed water: Wastewater that becomes suitable for beneficial use as
a result of treatment.
6. Supplier: The party that supplies material or services. A supplier may or
may not be the manufacturer.
7. Tamper-evident packaging: Packaging having one or more indicators
or barriers to entry that, if breached or missing, can reasonably be expected to
provide visible evidence to the purchaser that tampering has occurred. The tamper­
evident features of the packaging shall be designed to, and shall, remain intact
when handled in a reasonable manner during manufacture, storage, shipment, and
delivery to the purchaser. Properly constructed, labeled, and closed multiwall paper
bags and fiber drums constitute effective forms of tamper-evident packaging.
8. "Wastewater: A combination of the liquid and water-carried waste from
residences, commercial buildings, industrial plants, and institutions, together with
any groundwater, surface water, and stormwater that may be present.

* NSF International, 789 North Dixboro Road, Ann Arbor, Ml 48105.

t American National Standards Institute, 25 West 43rd Street, Fourth Floor, New York, NY 10036.
* Standards Council of Canada, 55 Metcalfe Street, Suite 600, Ottawa, ON KIP 6L5 Canada.
 AMMONIUM SULFATE 3

SECTION 4: REQUIREMENTS

Materials shall comply with the requirements of the Safe Drinking Water
Act and applicable federal, state, provincial, territorial, or other authoritative
regulations for potable water, wastewater, and reclaimed water systems.

Sec. 4.1 Physical Requirements

4.1.1 Form. The material supplied according to this standard shall be
homogeneous and in a fine-crystalline form suitable for feeding with dry feeders.
It shall be free from lint, chips, or other foreign matter.
4.1.2 Anticaking agent. The purchaser may require the addition of a
small amount of amorphous silica to the material. The amount of amorphous silica
added shall be sufficiently small so that it will not lower the percent of available
ammonia below the amount specified in Sec. 4.2.2. No surface-active agent or
detergent in any form shall be used as an anticaking agent.

Sec. 4.2 Chemical Requirements

The ammonium sulfate supplied shall meet the following requirements:
4.2.1 Moisture content. The moisture content shall not exceed
0.25 percent.
4.2.2 Available ammonia content. The available ammoma content,
expressed as NH3, shall not be less than 25 percent.
4.2.3 Free-acid content. The free-acid content, expressed as H2S04, shall
not exceed 0.15 percent.

Sec. 4.3 Impurities*

4.3.1 General impurities. The material supplied in accordance with this
standard shall contain no soluble inorganic or organic substances in quantities
capable of producing deleterious or injurious effects to the health of those
consuming water that has been properly treated with the material.
4.3.2 Specific impurities. The ammonium sulfate shall not contain
specific impurities in excess of the following limits (by weight):
4.3.2.1 Pyridine-50 mg/kg.
4.3.2.2 Ether-soluble matter-30 mg/kg.
4.3.2.3 Cyanide-none detectable with the analytical method described in
Sec. 5.2.8.

* See Sec. LC of the foreword.

4 AWWA 8302-23

4.3.2.4 Caprolactam-0.2 percent by weight.

4.3.3 Taste and odor. The material shall contain no impurity that will
produce an unpleasant taste or odor in the water, either in the absence of chlorine
or in combination with chlorine in concentrations normally required for treatment
of a water supply.
4.3.4 Product certifications. The material is a direct additive used in the
treatment of potable water. This material should be certified as suitable for contact
with, or treatment of, drinking water by an accredited certification organization
in accordance with NSF/ANSI/CAN 60. Evaluation shall be accomplished in
accordance with requirements that are no less restrictive than those listed in NSF/
ANSI/CAN 60. Certification shall be accomplished by a certification organization
accredited by the American National Standards Institute.

SECTION 5: VERIFICATION

Sec. 5.1 Sampling

Sampling shall be conducted in accordance with this section of the standard.
Each sample container shall be labeled to identify it and shall be signed by the
sampler. A chain-of-custody form shall accompany all samples and shall be properly
completed by the individuals collecting samples.
5.1.1 Sampling point. Samples shall be taken at the point of destination.
5.1.2 Amount of shipment to be sampled. If the material is packaged, 5
percent of the packages shall be sampled. No sample shall be taken from a broken
package. In the case of bulk shipments, a composite sample should be taken from
each truck or railroad car carrying the material.
5.1.3 Composite sample from bulk shipments. A composite sample from
bulk shipments will include a single grab sample from near the center of each
sector or bay of the shipping vessel. A minimum of three grab samples will be
taken. Five or more grab samples, depending on shipment size, are recommended.
5.1.4 Sampling device. Ammonium sulfate may be sampled using a
sampling tube that is at least % in. (19 mm)* in diameter. The sample may be taken
from bulk shipments in trucks or railroad cars or from packages. If the ammonium

* Metric conversions given in this standard are direct conversions of US customary units and are not those specified in
International Organization for Standardization (ISO) standards.
 AMMONIUM SULFATE 5

sulfate is handled by conveyor or elevator, a mechanical sampling arrangement may

be used.
5.1.5 Sample size. A gross sample weighing at least 10 lb (4.5 kg) shall
be taken. It shall be thoroughly mixed and divided to provide three 1-lb (0.45-kg)
material samples. These shall be sealed in airtight, moisture-proof glass containers.
Each sample container shall be labeled, and the label shall be signed by the sampler.
5.1.6 Sample distribution. One of the sealed material samples is for use
by the purchaser for testing in accordance with Sec. 5.2 of this standard. The
remaining two material samples are for use in accordance with Sec. 5.3 of this
standard, if needed.

Sec. 5.2 Test Procedures

5.2.1 Sampling and /,aboratory examination. Sampling shall be conducted
in accordance with Sec. 5.1 of this standard. The laboratory examination of the
sample by the purchaser shall be completed within 5 days after receipt of shipment.
5.2.1.1 Test samples. Test samples shall be obtained from the sealed
material samples delivered to the laboratory. Material samples shall be unsealed
only when it is necessary to remove quantities of the material for testing.
5.2.1.2 Sample preparation. The material sample shall be thoroughly
mixed and divided to provide a test sample of approximately 100 g. The test sample
shall be stored in an airtight glass container. The sample container shall be unsealed
only when it is necessary to remove quantities of the material for testing. This shall
be accomplished quickly to avoid change in moisture content. The test sample
shall then be resealed for future use.
5.2.1.3 Sample retention. Test samples shall be retained for at least
30 days after the date of receipt before they are discarded.
5.2.1.4 Test procedures. Methods of testing ammonium sulfate shall
conform to the procedures presented in the following sections. The purchaser may
suggest alternative procedures. In any case of conflict, the methods of this standard
shall prevail.
5.2.2 Test procedure for moisture.
5.2.2.1 Procedure. Accurately weigh 10 g (to the nearest 1 mg) of the
sample into a short weighing bottle, then dry to constant weight in an oven at
103°C.
5.2.2.2 Calculation.

loss in weight, in grams

percent moisture = x I 00 (Eq 1)
weight of sample, in grams
6 AWWA 8302-23

5.2.3 Test procedure for available ammonia-formaldehyde method

5.2.3.1 Reagents.
1. 1.0 N sodium hydroxide, carbonate free.
2. 30 percent solution of formaldehyde that has been neutralized with
sodium hydroxide using phenolphthalein indicator. (This must be freshly prepared.)
3. Methyl orange indicator, aqueous solution.
5.2.3.2 Procedure.
1. Dissolve 1.0 g of the sample in boiled and cooled deionized water and
neutralize the acidity with sodium hydroxide to the methyl orange indicator end
point. The amount of sodium hydroxide is not recorded.
2. Add 5 mL formaldehyde (Sec. 5.2.3.1 [item 2]) and gently shake several
times.
3. Titrate with 1.0 N sodium hydroxide to the phenolphthalein indicator
end point.
5.2.3.3 Calculation.

mL 1.0NNaOH x 0.01703
percentNH3 = x 1OO (Eq 2)
weight of sample, in grams

5.2.4 Test procedure for available ammonia-alternative method

5.2.4.1 Reagents.
1. 1.0 N sodium hydroxide.
2. 1.0 N sulfuric acid.
3. 0.1 N sodium hydroxide.
4. Ammonia-free deionized water.
5. Methyl red indicator.
5.2.4.2 Procedure.
1. Accurately weigh 2.5 g of the sample of ammonium sulfate and put in a
Kjeldahl flask fitted with a spray trap and suitable condenser. Add 150 mL deionized
water (Sec. 5.2.4.1 [item 4]) and 15 mL 1.0 N sodium hydroxide (Sec. 5.2.4.1
[item 1]).
2. When the sample is completely dissolved, distill at least 100 mL from the
Kjeldahl flask into 40 mL 1.0 N sulfuric acid (Sec. 5.2.4.1 [item 2]), keeping the
delivery tube just under the receiving liquid.
3. Titrate the distillate with 0.1 N sodium hydroxide (Sec. 5.2.4.1 [item 3])
to the methyl red indicator end point.
5.2.4.3 Calculation.
 AMMONIUM SULFATE 7

mL 1.0N H2S04 - ( mL 0.1NNaOH x 0.1)

percentNH3 = x 0.01703 x 100 (Eq 3)
weight of sample, in grams

5.2.5 Test procedure for ether-soluble matter.

5.2.5.1 Reagent.
1. Anhydrous ethyl ether.
5.2.5.2 Procedure.
1. Accurately weigh 25 g of the sample to the nearest 0.01 g after drying for
2 h at 103°C.
2. Extract for 2 h in a soxhlet extractor using 25-30 mL anhydrous ethyl
ether (Sec. 5.2.5.1 [item 1]).
3. Dry the residue in a moisture-free atmosphere to constant weight.
5.2.5.3 Calculation.

weight of ether-soluble residue, in grams

percent ether-soluble matter = x 100 (Eq 4)
weight of sample, in grams

5.2.6 Test procedure for free acid.

5.2.6.1 Reagents.
1. 0.1 N sodium hydroxide.
2. Methyl red indicator.
5.2.6.2 Procedure.
1. Dissolve 24.5 g of sample in 100 mL deionized water and filter into a
500-mL flask.
2. Rinse the beaker and wash the filter with not more than 50 mL water.
3. Add four drops of methyl red indicator (Sec. 5.2.6.1 [item 2]) and, if
the solution has a reddish tint, titrate with 0.1 N sodium hydroxide (Sec. 5.2.6.1
[item 1]) added dropwise with constant shaking until a yellowish tint develops.
5.2.6.3 Calculation.

percent free acid ( as H2S04) = mL 0.1NNaOH x 0.02 x 100 (Eq 5)

5.2.7 Test procedure for pyridine.

5.2.7.1 Reagents.
1. 1.0 N sodium hydroxide.
2. 1.0 N sulfuric acid.
3. 0.1 N sodium hydroxide.
4. 0.1 N sulfuric acid.
8 AWWA 8302-23

5. Sodium hypobromite solution. Dissolve 100 g sodium hydroxide in

800 mL deionized water and cool; add 25 mL liquid bromine and shake until
dissolved; make up to 1 L. This solution must be prepared just before the time of
use.
CAUTION: Liquid bromine volatilizes readily. The vapor is highly corrosive and

extremely irritating to the mucous membrane when inhaled. If the liquid comes in
contact with skin, it produces severe burns that are difficult to heal. When working
with this element in the laboratory, the analyst should use a well-ventilated hood
and take any other protective measures necessary.
6. Methyl red indicator.
5.2.7.2 Apparatus.
1. Ammonia distillation apparatus.
5.2.7.3 Procedure.
1. Dissolve 50.0 g of the sample in 150 mL deionized water in a 1-L distilling
flask and add two drops methyl red indicator. Add 1.0 N sodium hydroxide
(Sec. 5.2.7.1 [item 1]) to the end point and then add 5 mL in excess.
2. Distill for 30 min, using glass beads, into a 1-L flask containing 10 mL
1.0 N sulfuric acid (Sec. 5.2.7.1 [item 2]) in 100 mL deionized water. It is important
to keep the condenser cool.
3. To the cooled distillate, add about 100 mL sodium hypobromite solution
(Sec. 5.2.7.1 [item 5]) and shake well.
4. Distill as much as possible, using glass beads, into a 500-mL flask
containing 10 mL 0.1 N sulfuric acid, being careful to keep the receiver cool.
5. Titrate with 0.1 N sodium hydroxide using methyl red indicator
(Sec. 5.2.7.1 [item 6]).
5.2.7.4 Calculation.

mLO.lN H2S04-mLO.lNNaOH
percent pyn. d.me= x O.OO7 9 x 1OO (Eq 6)
weight of sample, in grams

5.2.8 Test procedure for cyanide.

5.2.8.1 Reagents.
1. 50 percent solution of sodium hydroxide.
2. 10 percent solution of ferrous sulfate.
3. 10 percent solution of ferric chloride.
4. 1 :3 sulfuric acid, by volume.
5.2.8.2 Procedure.
 AMMONIUM SULFATE 9

1. Dissolve 2 g of the sample in a minimum amount of water in a test tube

and then add a few drops of the sodium hydroxide solution (Sec. 5.2.8.1 [item 1]).
2. Add one drop ferrous sulfate solution (Sec. 5.2.8.1 [item 2]) and one
drop ferric chloride solution (Sec. 5.2.8.1 [item 3]) and shake.
3. Add 3 mL of the 1:3 sulfuric acid (Sec. 5.2.8.1 [item 4]). A blue color
will develop if cyanide is present.
5.2.9 Test procedure for caprolactam-liquid-liquid extraction and gas
chromatography method.
5.2.9.1 Reagents.
1. Methylene chloride (dichloromethane), gas chromatography (GC), or
high-pressure liquid chromatography (HPLC) grade.
2. Caprolactam, 99 percent minimum purity.
5.2.9.2 Apparatus.
1. 40-mL vials used for volatile organics analysis.
2. Vial shaker apparatus.
3. Autosampler storage vials.
4. A suitable gas chromatograph and accessories, having an electronic
readout of the integrated peak area.
5.2.9.3 Procedure.
1. Dissolve 38-40 g of the dry salt in 65-70 g deionized water. Record the
salt weight to 0.01 g and the total solution weight to 0.1 g.
2. Weigh a 10-g aliquot of solution (to 0.01 g) into a 40-mL vial. Add
5.0 mL methylene chloride (Sec. 5.2.9.1 [item 1]) and seal the vial. Place the vial
in a shaker for 20 min.
3. After shaking and phase separation, pipette 1.0 mL of the methylene
chloride extract through a small drying tube filled with anhydrous sodium sulfate
for removing residual water. Then transfer the dried extract into a small autosampler
vial.
4. Make up one or more standard solutions of caprolactam in methylene
chloride. Calibrate the gas chromatograph for the retention time of caprolactam
and its concentration versus peak area.
5. Inject a microliter portion of the shaken extract into the gas
chromatograph. Obtain the retention time and peak area for the caprolactam peak.
Determine the caprolactam concentration in the extract in micrograms/milliliter
from the ratio of its peak area to the calibrated peak area.
5.2.9.4 Calculations. Total caprolactam in sample based on the GC peak:
10 AWWA 8302-23

( µg/mL ) 5.0 mL
----6 ---
x
x solution weight (g) = total grams caprolactam in dry salt sample (Eq 7)
[aliquot weight (g)] x 10

caprolactam in salt (g)

percent caprolactam = x 100 (Eq 8)
dry salt sample weight (g)

5.2.10 Test procedure for caprolactam-alternative method The caprolactam

in a sample of dry ammonium sulfate can also be analyzed by HPLC. An ion
chromatograph is used with a commercial variety of a C18 reverse phase column. A
dilute stock solution of the dry salt sample is made up, and a microliter-size aliquot
system is calibrated with known caprolactam standards. Calibration can also be
made by running aliquots of the unknown sample that have been spiked with
known amounts of caprolactam, which is called the standard additions method.
The choice of hardware and operational procedure will vary among laboratories.
An acceptable HPLC system will have sufficient resolution and accuracy for the
expected levels of caprolactam. It should also be recalibrated frequently, preferably
for each new sample.

Sec. 5.3 Notice ofNonconformance

If the ammonium sulfate delivered to the purchaser does not meet the
chemical, physical, safety, or security requirements of this standard, a notice
of nonconformance shall be provided by the purchaser to the supplier within
10 days after receipt of the shipment at the point of destination. The results of
the purchaser's test shall prevail unless the supplier notifies the purchaser that a
retest is desired within five days after receipt of the notice of nonconformance.
On receipt of the request for a retest, the purchaser shall forward one of the sealed
samples taken according to Sec. 5.1 to the supplier. In the event that the test results
obtained by the supplier on retesting do not agree with the test results obtained by
the purchaser, the other 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.
Material not complying with the requirements of this standard and the
purchaser's documents may be rejected. Replacement and retesting shall be
accomplished in accordance with the purchaser's documents.
Because the exact concentration of the active ingredient in specific shipments
of some materials can vary within an acceptable range (thereby conforming to the
 AMMONIUM SULFATE 11

standard), the purchase documents between purchaser and supplier should address
treatment of concentration variation.

SECTION 6: DELIVERY

Sec. 6.1 Marking*

6.1.1 Required. Each shipment of material shall be identified as to
product, grade, net weight, name and address of the manufacturer, and the
brand name. Packages or containers shall show a lot number and identification of
manufacturer when shipped in bulk. All markings on packages, containers, or bulk
shipments shall conform to applicable laws and regulations, including requirements
established by the US Occupational Safety and Health Administration (OSHA).
6.1.2 Optional. Packages may also bear the statement "Guaranteed by
(name of manufacturer) to meet the requirements of AWWA B302, Standard for
Ammonium Sulfate,'' provided that the requirements of this standard are met.

Sec. 6.2 Packaging and Shipping

6.2.1 Containers. Ammonium sulfate shall be shipped in 50-lb (23-kg)
or 100-lb (45-kg) multiwall paper bags, 400-lb (180-kg) fiber drums, or other
containers specified by the purchaser. At the purchaser's request, it may also be
shipped in bulk in paper-lined boxcars, in covered hopper or Airslide railroad cars,
or in trucks suitable for shipping dry bulk chemicals.
6.2.2 Net weight. The net weight of packages shall not deviate from the
recorded weight by more than ±2.5 percent. Any exception taken in regard to the
weight of the material received shall be based on a deviation from the certified unit
weight of not less than 5 percent of the packages shipped, selected at random from
the entire shipment.
6.2.3 Security requirements for nonbulk shipments. Packaged product
shall be stored, shipped, and delivered in tamper-evident packaging as defined in
Section 3 (item 7), or an alternative method or methods may be agreed on by
the manufacturer and purchaser that provide a reasonable assurance of protection
against tampering.

* Governmental packaging and marking references reflect US requirements. Users of this standard outside the United
States should verify applicable local and national regulatory requirements. Because of frequent changes in these
regulations, all parties should remain informed of possible revisions. Provisions of the purchaser's documents should
not preclude compliance with applicable regulations.
12 AWWA 8302-23

6.2.4 Security requirementsfor bulk shipments. Bulk quantities of product

shall be secured by employing one of the following security measures (or a
combination of measures):
6.2.4.1 Seals. Bulk quantities of product may be sealed with a uniquely
numbered tamper-evident seal(s). The seal numbers shall be recorded and disclosed
on shipping documents such as the bill of lading. Seals shall be inspected upon
receipt of product by the purchaser, and evidence of tampering or removal should
be reported to the carrier and supplier.
6.2.4.2 Chain of custody. A continuous chain of custody shall be
maintained between the manufacturer and the purchaser during storage and
shipment if so specified by the purchaser.
6.2.4.3 Alternative method. An alternative method or methods agreed on
by the manufacturer and purchaser that provide reasonable assurance of protection
against tampering.

Sec. 6.3 Affidavit of Compliance or Certified Analysis

The purchaser may require either (1) an affidavit from the manufacturer that
the material provided complies with applicable requirements of this standard or (2)
a certified analysis of the material at the time of delivery detailing the desired items.
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1 P 8.SC 42302-23 5/23 QI