Awwa b403-98
Awwa b403-98
Awwa b403-98
ANSI/AWWA B403-98
(Revision of ANSI/AWWA B403-93)
AWWA STANDARD
FOR
ALUMINUM SULFATELIQUID,
GROUND, OR LUMP
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Standard may be revised or withdrawn at any time.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.
ii
Copyright 1999 American Water Works Association, All Rights Reserved.
Committee Personnel
The AWWA Subcommittee on Aluminum Sulfate, which developed this standard,
had the following personnel at the time:
The AWWA Standards Committee on Iron Salts, Aluminum Salts, and Related
Coagulant Aids, which reviewed and approved this standard, had the following
personnel at the time of approval:
Consumer Members
* Alternate
Liaison, nonvoting
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Copyright 1999 American Water Works Association, All Rights Reserved.
J.J. Gemin, Proctor and Redfern Ltd., Kitchener Ont. (AWWA)
R.D. Harriger, Alexandria Bay, N.Y. (AWWA)
J.F. Myatt,* Proctor & Redfern Ltd., London, Ont. (AWWA)
J.W. Patterson, Patterson Associates Inc., Chicago, Ill. (AWWA)
E.S. Ralph, Standards Engineer Liaison, Denver, Colo. (AWWA)
R.R. Smith, Austell, Ga. (AWWA)
Producer Members
* Alternate
Liaison, nonvoting
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Copyright 1999 American Water Works Association, All Rights Reserved.
Contents
All AWWA standards follow the general format indicated subsequently. Some variations from this format may be
found in a particular standard.
Foreword 4 Requirements
I Introduction........................................ vii 4.1 Physical Requirements......................... 2
I.A Background......................................... vii 4.2 Chemical Requirements ....................... 3
I.B History ................................................ vii 4.3 Impurities.............................................. 3
I.C Acceptance ......................................... viii 5 Verification
II Special Issues ....................................... ix
5.1 Sampling ............................................... 4
II.A Safety and Spill Control ...................... ix
5.2 Test ProceduresGeneral ................... 4
III Use of This Standard........................... ix
5.3 Specific Gravity .................................... 5
III.A Purchaser Options and
5.4 Water-Insoluble Matter ....................... 5
Alternatives....................................... ix
5.5 Total Soluble Alumina and
III.B Modification to Standard...................... x
Aluminum .......................................... 5
IV Major Revisions..................................... x
5.6 Total Water-Soluble Iron ..................... 8
V Comments.............................................. x
5.7 Ferric Iron............................................. 9
5.8 Ferrous Iron .......................................... 9
Standard
5.9 Basicity or Free Acid.......................... 10
1 General 5.10 Total Alumina Alternative Method... 11
1.1 Scope ...................................................... 1 5.11 Basis for Rejection.............................. 12
1.2 Purpose .................................................. 1
6 Delivery
1.3 Application............................................. 1
6.1 Marking............................................... 12
2 References ........................................... 1 6.2 Packaging and Shipping .................... 13
6.3 Affidavit of Compliance...................... 13
3 Definitions........................................... 2
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Copyright 1999 American Water Works Association, All Rights Reserved.
This page intentionally blank.
I. Introduction.
I.A. Background. Coagulation of suspended and colloidal particles in water
using various forms of aluminum sulfate has been known since the 17th century.
Although historical details are lacking, in the early days of water purification by
coagulation, lump or slab forms of aluminum sulfate were dissolved and added to the
water in solution form. Sommerville, N.J., was probably the first utility in the United
States serving potable water to use this treatment method on a more or less
continuous basis. Shortly thereafter, numerous plants adopted this method, including
the Hackensack (N.J.) Water Company and those of the former American Water
Works and Electric Company.
The terms filter alum, papermakers alum, and commercial alum all refer to the
same chemical: aluminum sulfate. Aluminum sulfate, as produced in tonnage
quantities, has the formula Al2(SO4)3 nH2O, where n is approximately 14 waters of
crystallization instead of 18, which is the true crystalline form. The purpose of
producing a form of aluminum sulfate that has 14 waters of crystallization is twofold.
First, it is stable and gains or loses water slowly under adverse storage conditions.
Second, aluminum sulfate having 14 waters of crystallization is approximately
12 percent stronger than aluminum sulfate having 18 waters of crystallization. Using
the more concentrated form of the chemical reduces the tonnage to be handled,
reduces chemical storage requirements, and saves the consumer transportation costs.
Several other dry alums are used in treating swimming pool water and certain
industrial waters. These products are true alums, which are double salts containing
24 waters of crystallization, such as ammonia alum Al2(SO4)3 (NH4)2SO4 24H2O
and potash alum Al2(SO4)3 K2SO4 24H2O. These specialty alums are excellent
coagulants, but have a lower Al2O3 content and are not widely used compared with
aluminum sulfate. Commercial liquid alum is shipped as a relatively clear, stable
solution that contains up to 48.5 percent by weight dry product. In recent years,
manufacturers have built production plants in areas of high consumption and now
the United States has many alum-producing plants.
Aluminum sulfate is prepared from aluminum hydroxide, alumina trihydrate, or
alumina-bearing ores, such as clay and bauxite. The aluminum ore is ground to a
required fineness and digested with sulfuric acid at elevated temperatures. Insoluble
materials are removed by sedimentation. The supernatant solution is either decanted
and sold in liquid form or concentrated and allowed to crystallize into a solid, dry,
hydrated product. The aluminum oxide content of the liquid is limited to about
8 percent Al2O3 to avoid crystallization in transit and storage. The solid, dry,
hydrated product usually contains 17 percent Al2O3.
Liquid alum may be received and stored in corrosion-resistant tanks and
transferred through appropriate liquid-metering devices directly into the water at
the desired point of application.
I.B. History. A specification for Sulphate of Alumina was published in 1925
by the American Water Works Association (AWWA) in its Water Works Practice Manual.*
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Copyright 1999 American Water Works Association, All Rights Reserved.
On June 25, 1942, AWWA adopted the Emergency Alternate Specifications for
Sulphate of Alumina, which relaxed some provisions and allowed the chemical to be
made from lower-quality raw materials. (As a wartime measure, higher-quality
bauxite had been diverted to the aluminum-metals industry.) In 1952, the committee
upgraded the standard under the guidance of J.E. Kerslake, with Paul Tamer acting
as referee for the comments from producers and consumers. The standard was
revised in 1958 to include liquid aluminum sulfate. Other revisions were made in
1964, 1969, 1970, 1982, 1988, and 1993.
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 Environ-
mental 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 ChemicalsHealth
Effects, and ANSI/NSF 61, Drinking Water System ComponentsHealth Effects.
Various certification organizations may be involved in certifying products in
accordance with ANSI/NSF 60 (61). Individual states or local agencies have authority
to accept or accredit certification organizations within their jurisdiction. Accredita-
tion 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 B403-98 addresses additives requirements in Sec. 4.3 of the standard.
The transfer of contaminants from chemicals to processed water or the residual solids
is becoming a problem of greater concern. The language in Sec. 4.3.3 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 ChemicalsHealth 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.
*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 48106.
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Copyright 1999 American Water Works Association, All Rights Reserved.
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 and Spill Control. Aluminum sulfate is a buffered acidic solution
that causes irritation when it comes in contact with the eyes, skin, or mucous
membranes. Protective clothing and equipment should be used when handling liquid
alum. Good ventilation, good housekeeping procedures, and personal cleanliness are
also recommended.
Protective equipment. Dry aluminum sulfate dust can cause irritations to the
respiratory system and eyes. Dust masks, goggles, and gloves are recommended for
persons working in the presence of dry aluminum sulfate dust.
Normal precautions should be used to prevent spraying or splashing liquid
alum. Face shields should be worn to protect the eyes. Outer coverings, such as vinyl
or rubber rain jackets and pants, may be used to protect clothing from liquid alum.
First aid. Aluminum sulfate should be flushed from the eyes using copious
amounts of water. If irritation persists, a physician should be consulted promptly.
Aluminum sulfate should be washed from the skin with copious amounts of water.
For additional safety information, refer to material safety data sheets (MSDS)
available from the chemical supplier or manufacturer.
Spill-control considerations. Outdoor storage tanks should be suitably diked or
otherwise provided with an adequate means of secondary containment. Appropriate
secondary containment measures should be taken to prevent spills or leaks from
indoor storage tanks and tank-car or tank-truck unloading stations from entering
sewers or other channels that discharge directly to a water body or a municipal
sewage system.
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
standards provisions are suitable for and compatible with that users intended
application.
III.A. Purchaser Options and Alternatives. When purchasing aluminum sul-
fate under the provisions of this standard, the following items should be covered in
the purchasers specifications:
1. Standard usedthat is, ANSI/AWWA B403, Standard for Aluminum
SulfateLiquid, Ground, or Lump, of latest revision.
2. Affidavit of compliance, certified analysis, or both, if required (Sec. 6.3).
3. Type of aluminum sulfate requiredliquid, ground, or lump (Sec. 4).
Standard practice is to order liquid alum on a dry basis by specifying the quantity
of aluminum sulfate as weight of dry chemical in a water solution.
4. Quantity required and method of packaging and shipping (Sec. 6).
5. If less-than-carload quantities of liquid alum are ordered, the type and size
of container required (Sec. 6.2.2.2).
6. If bulk shipments are to be accompanied by weight certificates or
certificates issued by certified weighers (Sec. 6.2.4).
7. If basic or acidic alum is required (Sec. 4.2.2).
8. Whether the recommended compliance with ANSI/NSF Standard 60,
Drinking Water Treatment ChemicalsHealth Effects, is to be required. If this
certification is to be required, the purchasers specifications shall read, This material
shall be certified as suitable for contact with or treatment of drinking water by an
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Copyright 1999 American Water Works Association, All Rights Reserved.
accredited certification organization in accordance with ANSI/NSF Standard 60,
Drinking Water Treatment ChemicalsHealth Effects.
9. In the event that an analysis by a referee laboratory is required, the
assignment of testing costs should be addressed (Sec. 5.11.1).
III.B. Modification to Standard. Any modification of the provisions, defini-
tions, or terminology in this standard must be provided in the purchasers
specifications.
IV. Major Revisions. Major revisions to the standard in this edition include
the following:
1. The format has been changed to AWWA standard style.
2. The acceptance statement (Sec. I.C) has been changed to approved wording.
3. A new section on product certifications (Sec. 4.3.3) has been added.
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) 795-1440, or write to the department at 6666 W. Quincy Ave.,
Denver, CO 80235.
x
Copyright 1999 American Water Works Association, All Rights Reserved.
American Water Works Association
ANSI/AWWA B403-98
(Revision of ANSI/AWWA B403-93)
ALUMINUM SULFATELIQUID,
GROUND, OR LUMP
SECTION 1: GENERAL
Sec. 1.1 Scope
This standard covers purified aluminum sulfate in liquid, ground, or lump form,
for use in water treatment.
Sec. 1.2 Purpose
The purpose of this standard is to provide purchasers, manufacturers, and
suppliers with the minimum requirements for aluminum sulfate, including physical,
chemical, packaging, shipping, and testing requirements.
Sec. 1.3 Application
This standard can be referenced in specifications for purchasing and receiving
aluminum sulfate, and can be used as a guide for testing the physical and chemical
properties of aluminum sulfate samples. The stipulations of this standard apply
when this document has been referenced and then only to aluminum sulfate used in
water supply service.
SECTION 2: REFERENCES
This standard references the following documents. In their latest editions, they
form a part of this standard to the extent specified in this standard. In any case of
conflict, the requirements of this standard shall prevail.
1
Copyright 1999 American Water Works Association, All Rights Reserved.
2 AWWA B403-98
ASTM* E11Standard Specification for Wire Cloth and Sieves for Testing
Purposes.
ASTM E200Standard Practice for Preparation, Standardization, and Storage
of Standard and Reagent Solutions for Chemical Analysis.
Standard Methods for the Examination of Water and Wastewater. APHA,
AWWA, and WEF. Denver, Colo. (19th ed., 1995).
SECTION 3: DEFINITIONS
The following definitions shall apply in this standard:
1. Acidic alum: Acidic alum contains sulfuric acid, which is not combined as
aluminum sulfate (expressed as free H2SO4).
2. Aluminum sulfate: The product of the reaction between sulfuric acid and a
mineral rich in aluminum, such as bauxite.
3. Basic alum: Basic alum contains water-soluble aluminum, which is not
combined as aluminum sulfate (expressed as free Al2O3).
4. Manufacturer: The party that manufactures, fabricates, or produces
materials or products.
5. Purchaser: The person, company, or organization that purchases any
materials or work to be performed.
6. Purified aluminum sulfate: Purified ground or lump aluminum sulfate that
complies with the provisions of this standard and contains water-insoluble matter not
exceeding 0.5 percent.
7. Supplier: The party that supplies materials or services. A supplier may or
may not be the manufacturer.
SECTION 4: REQUIREMENTS
Sec. 4.1 Physical Requirements
Aluminum sulfate is the product of the reaction between sulfuric acid and a
mineral rich in aluminum, such as bauxite. Solid aluminum sulfate shall be dry,
clean, and shall be lump or ground, as specified. Liquid alum is a nearly saturated
solution of aluminum sulfate.
4.1.1 Lump aluminum sulfate. Lump aluminum sulfate shall range in size so
that 100 percent passes through a 3-in. (7.62-cm) ring and at least 75 percent shall
be retained on a 1 2 -in. (13-mm) sieve.**
*American Society for Testing and Materials, 100 Barr Harbor Dr., West Conshohocken, PA
19428-2959.
American Public Health Association, 1015 5th St. N.W., Washington, DC 20005.
Water Environment Federation, 601 Wythe St., Alexandria, VA 22314-1994.
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.
**ASTM E11.
*ASTM E11.
See Sec. I.C of foreword.
There are a number of water treatment plants in which aluminum sulfate of a higher iron
content can be used without increasing the iron content of the treated water. If a purchaser
determines that aluminum sulfate having a higher iron content can be used satisfactorily and,
therefore, specifies a higher permissible iron content, aluminum sulfate with a higher iron
content may be furnished.
American National Standards Institute, 11. W. 42nd St., New York, NY 10036.
**NSF International, 3475 Plymouth Rd., Ann Arbor, MI 48106.
SECTION 5: VERIFICATION
Sec. 5.1 Sampling
5.1.1 Sampling point. Samples shall be taken at the point of destination.
5.1.2 Lump or ground aluminum sulfate.
5.1.2.1 If the aluminum sulfate is handled by conveyor or elevator, a mechanical
sampling arrangement may be used.
5.1.2.2 If the aluminum sulfate is packaged, 5 percent of the packages shall be
sampled. No sample shall be taken from a broken package.
5.1.2.3 In sampling lump material in bulk cars, sampling points shall be
selected uniformly over the surface of the bulk material. Whenever possible, a
minimum of 10 points at regular intervals shall be selected. At least 7 lb (3.2 kg)
(about a shovelful) shall be taken at each point.
5.1.2.4 The sample must include a proportionate amount of lumps and fines.
Overburden should be removed as necessary to obtain access to representative material.
5.1.2.5 Ground aluminum sulfate in bulk carload shipments or in packages
should be sampled using a sampling tube or other effective device that measures at
least 3 4 in. (19 mm) in diameter.
5.1.2.6 The gross sample, weighing at least 50 lb (23 kg), shall be crushed, if
necessary, and mixed thoroughly and divided to provide three 1-lb (0.5-kg) samples.
These samples shall be sealed in airtight, moistureproof glass containers.
5.1.2.7 The 1-lb (0.5-kg) sample of lump aluminum sulfate delivered to the
laboratory shall be quartered to approximately 100 g. This amount shall be reduced
by mechanical grinding or grinding rapidly in a mortar by hand to such size that all
of it passes a No. 30 sieve.* After thorough mixing, this sample shall be stored in an
airtight glass container. Samples of ground aluminum sulfate are split in the same
way, except that the samples need not be reduced by further pulverizing. The
necessary amounts shall be weighed from the glass container rapidly to avoid change
in moisture content.
5.1.2.8 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.
5.1.3 Liquid alum.
5.1.3.1 Equal portions shall be taken at five equally spaced time intervals during
the unloading of the tank truck or railroad car. The total sample shall equal 2 qt (2 L).
5.1.3.2 The gross sample (2 qt [2 L]) should be thoroughly mixed, and three
1-pt (0.5-L) samples retained. They shall be sealed in airtight glass containers.
5.1.3.3 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.
Sec. 5.2 Test ProceduresGeneral
5.2.1 Laboratory examination. Laboratory examination by the purchaser of
one of the three samples shall be completed within five working days after receipt of
the shipment.
*ASTM E11.
5.2.2 Safety. Those unfamiliar with the hazards of any chemicals used in the
test procedures that follow should consult current manufacturers material safety
and health data sheets (MSDS) or other appropriate material safety and health
references.
Sec. 5.3 Specific Gravity
The specific gravity of aluminum sulfate solution may be determined with
reasonable accuracy by use of a hydrometer that meets or exceeds the ASTM
standards for 117-H, or by use of a specific-gravity balance or a pycnometer. The
aluminum sulfate manufacturer should furnish information showing percentage of
aluminum as Al or Al2O3 for aluminum sulfate solutions of different specific-gravity
readings.
Sec. 5.4 Water-Insoluble Matter
5.4.1 Procedure.
5.4.1.1 Place a glass-fiber filter disc in a Gooch crucible, dry at 105 to 110C,
cool in desiccator, and weigh to the nearest 0.001 g.
5.4.1.2 Weigh out 20 g of dry aluminum sulfate or 40 g of liquid alum to the
nearest 0.01 g. Dissolve the dry aluminum sulfate in approximately 150 mL of hot
distilled water and stir for a few minutes. Dilute the liquid alum in 150 mL of hot distilled
water and stir.
5.4.1.3 Filter through the prepared crucible. Wash the residue with hot
distilled water in at least three 25-mL rinses, or until the filtrate is free from
sulfates.*
5.4.1.4 Dry in an oven to constant weight (nearest 0.001 g) at 105 to 110C
and calculate the percentage of insoluble matter using the following formula:
weight of insoluble residue
-------------------------------------------------------------------------- 100 = % insoluble matter (Eq 1)
weight of sample
5.5.6 Sample preparation for standard alum liquor and iron-free alum liquor.*
5.5.6.1 To a 500-mL Erlenmeyer flask or 400-mL beaker, add 50 mL of water.
5.5.6.2 Fill a 1-cm3 disposable syringe to the 1-cm3 mark with the liquor
sample. Wipe the Luer tip of the syringe with tissue and weigh the syringe plus
sample to the nearest 0.1 mg.
5.5.6.3 Transfer the sample to the beaker or flask. Reweigh the syringe to the
nearest 0.1 mg and obtain the sample weight by difference.
5.5.6.4 Add two drops of 1:1 sulfuric acid and mix.
5.5.6.5 Continue with step 1 of the procedure (Sec. 5.5.8).
5.5.7 Sample preparation for all other alum products.
5.5.7.1 Calculate the size sample to be used, as follows:
* Where Al2O3 is 8.0 to 9.4 percent and free Al2O3 or free H2SO4 is less than 0.5 percent
11.5
grams sample = ---------------------------------------------------------------- (Eq 3)
expected % total Al 2 O 3
Weigh a sample of this size (0.1 g), weighing with an accuracy of 0.001 g.
Quantitatively transfer to a 400-mL beaker and dilute to about 300 mL with water.
5.5.7.2 Add sulfuric acid in the amounts specified below.
1. For an alum product containing no more than a few tenths of a percent of
either free Al2O3 or free H2SO4, add 18 to 20 drops of 1:1 sulfuric acid to the beaker.
2. For an acidified alum product, calculate the quantity of sulfuric acid to be
added as follows (see Sec. 5.5.10.1):
19 grams sample % H 2 SO 4 in sample
drops H 2 SO 4 = ----------------------------------------------------------------------------------------------------------------- (Eq 4)
5
drops H 2 SO4 =
19 + ( grams sample percent free Al 2 O 3 in sample 0.06 ) (Eq 5)
% Al 2 O 3 = (Eq 7)
% Al 2 O 3 and total Fe as Al 2 O 3 ( % total Fe as Fe 2 O 3 0.6385 )
5.5.10 Notes.
5.5.10.1 The computation given for the quantity of sulfuric acid to be added to
acidified alum solutions will result in the addition of 0 to 19 drops of the 1:1 acid for
alums being produced currently. If a particular computation should result in a small
negative value for the number of drops (that is, one to three), the number of drops to
be added is taken as zero. If a significant negative value (that is, four or more drops)
results from the computation, add three drops of 6N NaOH solution for each drop of
1:1 H2SO4 computed.
5.5.10.2 The aliquot of sample solution used for titration should contain 0.110
to 0.125 g of aluminum calculated as Al2O3. If too large a sample size is taken for the
test, the color change may occur when the first drop of zinc sulfate is added. In this
event, rerun the analysis using a 25-mL aliquot of the prepared sample solution.
5.5.10.3 The sample solution, the added standard excess EDTA solution, and
the ammonium acetate buffer solution are boiled together to ensure quantitative
complexation of the aluminum with EDTA. A boiling time of 2 to 3 min is adequate.
Close control over the volume of liquid is not required; however, do not let the sample
evaporate to dryness.
5.5.10.4 EDTA chelates with multivalent cations on a 1:1 basis. Thus, the
valence state of iron, for example, is of no consequence, and a correction is made only
for total Fe expressed as Al2O3.
Sec. 5.6 Total Water-Soluble Iron
5.6.1 Apparatus. Spectrophotometer.
5.6.2 Reagents.
5.6.2.1 Potassium thiocyanate (KCNS) solution, 10 percent by weight.
5.6.2.2 Sulfuric acid, 1:1 by volume or 18N. Carefully mix, while stirring, equal
volumes of sulfuric acid and water in a borosilicate glass (Pyrex) beaker. Allow to cool
to room temperature. NOTE: Always add acid to water.
5.6.2.3 Potassium permanganate (KMnO4), approximately 1.0 percent. Store
in an amber glass bottle. Shelf life is approximately 6 months.
5.6.2.4 Standard iron solution, 1.0 mg Fe/mL.
5.6.2.5 Standard iron solution, 0.10 mg Fe/mL. Prepare by dilution of 1.0 mg
Fe/mL standard. Include 10 mL 1:1 H2SO4 per litre of standard solution.
5.6.3 Calibration.
5.6.3.1 To a 100-mL volumetric flask, using a pipette, add 1.00 mL of 0.10 mg
Fe/mL standard iron solution, 50 mL of water, 10.0 mL of 1:1 sulfuric acid, and
1 percent potassium permanganate, drop by drop, to obtain a persistent pink color.
Add 10.0 mL of 10 percent potassium thiocyanate and dilute to the mark. Measure in a
spectrophotometer at 475 nm within 10 min against a blank. Prepare the blank
solution by transferring 10 mL of a 10 percent potassium thiocyanate solution and 10 mL
of 1:1 sulfuric acid to a 100-mL volumetric flask. Dilute to the mark with water and mix.
5.6.3.2 Repeat, using 2.00, 3.00, 4.00, and 5.00 mL of 0.10 mg Fe/mL standard
iron solution in successive flasks. Measure each within 10 min of preparation.
5.6.3.3 If the spectrophotometer is not direct-reading, plot the absorbance
versus milligrams of iron on rectangular coordinate paper or plot percent transmit-
tance versus milligrams of iron on semilog paper. Reducing the relationship to an
equation is preferable.
5.6.4 Procedure.
5.6.4.1 Weigh out (accurate to 0.01 g) 10 g of liquid alum or 5 g dry alum and
dilute to 1 L in a volumetric flask.
5.6.4.2 To a 100-mL volumetric flask, add 10.00 mL of sample solution, 50 mL
water, 10.0 mL of 1:1 sulfuric acid, and 1 percent potassium permanganate, drop by
drop, to obtain a persistent pink color.
5.6.4.3 Cool to room temperature.
5.6.4.4 Add 10.0 mL of 10 percent potassium thiocyanate and dilute to the mark.
5.6.4.5 Measure in a spectrophotometer at 475 nm within 10 min against a
blank.
5.6.4.6 This procedure is designed to determine iron in liquid alum in the
range of 0.1 to 0.7 percent Fe2O3. If the iron content is outside of this range, the
aliquot taken from the 1-L volumetric flask should be changed from the 10 mL stated
in the previous procedure. This will change B in the equation for calculating percent
Fe2O3 (see Sec. 5.7.2).
Sec. 5.7 Ferric Iron
5.7.1 Procedure. Use the procedure above for testing total iron, except do not
use the potassium permanganate.
5.7.2 Calculations.
( M ) ( B ) ( C ) ( 100 )
-------------------------------------------- = % iron as Fe 2 O 3 (as is) (Eq 8)
(W)(D )
Where:
M = milligrams iron
B = total volume of sample solution divided by portion used:
1,000 mL/10 mL = 100
C = conversion factor: Fe to Fe2O3 = 1.4297
W = weight of sample, in grams
D = conversion factor: sample weight in grams to milligrams = 1,000
Using the values given above, Eq 8 becomes:
( M ) ( 100 ) ( 1.4297 ) ( 100 ) ( M ) ( 14.297 )
---------------------------------------------------------------- = ---------------------------------- = % iron as Fe 2 O 3 (as is)
( W ) ( 1,000 ) (W)
*In this method, potassium hydroxide may be used as the alkali in place of sodium hydroxide
on an equivalent basis.
Hydrofluoric acid is an extremely dangerous and hazardous chemical capable of causing
serious injury or death. Users of this chemical must familiarize themselves with all the
necessary safety and handling precautions available from the chemical supplier.
amount of sulfuric acid added (that is, greater than 10 mL). The sample is neutral if
the sodium hydroxide back-titration is equal to the sulfuric acid added.
Sec. 5.10 Total Alumina Alternative Method
Refer to Analytic Methods for Atomic Absorption Spectrophotometry* when using
this procedure.
5.10.1 Reagents.
5.10.1.1 Deionized water.
5.10.1.2 25 percent potassium chloride solution. Dissolve 125 g of reagent-grade
potassium chloride KCl in 500 mL with deionized water in a 500-mL volumetric flask.
5.10.1.3 Concentrated, reagent-grade nitric acid, HNO3.
5.10.1.4 Stock aluminum standard, 1,000 mg/L as Al. Obtain premade from
Fisher Scientific Corporation, Pittsburgh, Pa., or equivalent.
5.10.1.5 Working Al standard solutions. Into a series of separate 100-mL
volumetric flasks, pipette 0.0, 1.0, 2.5, and 5.0 mL of the 1,000 mg/L stock Al
standard. Add 2.0 mL of 25 percent KCl solution and 1.0 mL of concentrated nitric
acid to each flask. Dilute to volume with deionized water and mix. These standards
have concentrations of 0, 10, 25, and 50 mg/L as Al, respectively.
5.10.2 Apparatus.
5.10.2.1 Atomic absorption spectrophotometer (AAS), Perkin Elmer 306 or
equivalent.
5.10.2.2 Aluminum hollow cathode lamp.
5.10.2.3 Volumetric flasks, assorted sizes.
5.10.2.4 Balance, accurate to 0.001 g.
5.10.2.5 Volumetric pipettes, assorted sizes.
5.10.3 Instrument operating conditions.
5.10.3.1 Wavelength: 309.3 nm.
5.10.3.2 Slit width: 0.7 nm.
5.10.3.3 Lamp energy: 15 milliamperes (mA).
5.10.3.4 Burner: N2O single slot, parallel.
5.10.3.5 Flame type: N2O-Acetylene oxidizing (lean, blue).
5.10.3.6 Gas-pressure settings: Follow manufacturers recommendations depend-
ing on the type of gas control in use.
5.10.4 Procedure.
5.10.4.1 Obtain the test sample and make any necessary dilutions with
deionized water to allow the final dilution to be in the linear working range of the
instrument (<50 mg/L as Al). Typically, the first dilution is 1:50. All sample weights
should be obtained to the nearest 0.001 g. Pipette 5.0 mL of above solution into a
100-mL volumetric flask for the second dilution.
5.10.4.2 Pipette 2.0 mL of 25 percent KCl solution and 1.0 mL of concentrated
HNO3 into the flask and dilute to 100 mL with deionized water. Mix well. Prepare a
blank by repeating this step in a clean and dry volumetric flask.
5.10.4.3 Optimize the instrumental parameters, such as wavelength, burner
position, lamp alignment, fueloxidant ratios, and nebulization rate, following
manufacturers instructions.
5.10.4.4 Aspirate and measure the absorbance of the blank and a set of
working standards solutions. The concentration range of the standards is 0 to 50 mg/L
as Al.
5.10.4.5 Aspirate and measure the absorbance of the diluted test-sample solutions.
5.10.4.6 Prepare a calibration curve by plotting on linear graph paper
absorbance versus concentration of Al in mg/L for the standards. Obtain the
concentration of Al in mg/L in the diluted test samples from sample absorbance
values and the corresponding concentrations on the calibration curve. Alternatively,
a curve can be fit to the data using a scientific calculator with linear regression
capability. Sample concentration can be read directly from some instruments with
automatic calibration.
5.10.5 Calculations.
5.10.5.1 Concentration in mg/L of Al in test sample:
mg/L as Al = (mg/L in diluted test sample) (D)
where D = any appropriate dilution factors
( mg/L as Al )
5.10.5.2 Percent Al = ----------------------------------
10, 000
5.10.5.3 Percent Al2O3 = (percent Al) (1.89)
5.10.6 Performance data.
5.10.6.1 Range: 0 to 50 mg/L as Al in aspirated solutions.
5.10.6.2 Precision. Sample deviation is 1.18 percent relative as determined
by three replicates of four samples by one operator.
Sec. 5.11 Basis for Rejection
5.11.1 Notice of nonconformance. If the aluminum sulfate delivered does not
meet the requirements of this standard, a notice of nonconformance must 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 purchasers tests shall prevail unless the
supplier notifies the purchaser within five working days after receipt of the notice of
complaint that a retest is desired. On receipt of the request for a retest, the
purchaser shall forward to the supplier one of the sealed samples taken according to
Sec. 5.1. If the results obtained by the supplier on retesting do not agree with the
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.
SECTION 6: DELIVERY*
Sec. 6.1 Marking
Each shipment of lump or ground material shall carry with it some means of
identification. The following information shall be legibly marked on each package,
drum, other container, or bulk shipment:
*Tank cars used in areas where air temperatures below 5F (15C) prevail should be provided
with insulation.