.. y

CHEMICAL TESTING METHODS

FOR COMPLYING WITH THE

DANGEROUS WASTE REGULATION

Chapter 173-303 WAC

STATE OF WASHINGTON

DEPARTMENT OF ECOLOGY

March 1982

I· .
1. Introduction

TABLE OF CONTENTS

1

2. Narrative of EPA Characteristic Testing

A.

B.

C.

D.

Ignit abili ty

Corrosivity - pH and Corrosiveness

Reactivity

E.P. Toxicity

1

2

2

3

3. Narrative of WDOE Persistence Testing

A.

B.

C.

Crude Sample Extraction

Halogenated Hydrocarbons

Polycyclic Aromatic Hydrocarbons

4

5

5

APPENDICES

--- ...

A.

B.

C.

D.

E.

F.

G.

Ignitabili ty

Corrosivity

Reactivity

EP Toxid ty

Crude Sample Extraction for Halogenated and

Polycyclic Aromatic Hydrocarbon Analysis

Halogenated Hydrocarbon Analysis

Polycyclic Aromatic Hydrocarbons

A-I

B-1

c-r

D-l

E-l

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I.

II.

.--. .... '

Introduction

This manual sets forth methods for chemical testing of suspected

dangerous wastes. Biological testing methods are set forth in "Biological Testing Methods" wnOE 80-12, October, 1980. This manual

is organized in two phases for each test method: (1) a narrative

description of the test method for the non-technical reader, and

(2) an appendix test method giving all the details for the practicing

chemist or laboratory conducting such tests. Sone appendix test methods

reference other methods because of copyright restrictions (as for ASTM)

or length (as for EPA analytical methods).

Within this framework, the manual describes Environmental Protection

Agency tests for ignitability, corrosivity, pH and extraction procedure

(EP) toxicity. In addition, it sets forth the Department of Ecology's

chemical tests for halogenated hydrocarbons and polycyclic aromatic

hydrocarbons.

Narrative of EPA Tests for Hazardous Waste Characteristics

Chapter 173-303 WAC requires all generators to test their waste for four

characteristics. These are igni tabili ty, cor ros ivi ty, reactivi ty, and

extraction procedure (EP) toxi city. The rationale for choice of these

characteristics are discussed in the Federal Register, May 19, 1980.

Most of the detailed test methods for this section are taken from the

EPA publication, "Test Methods for Evaluating Solid Waste - Physical

Chemical Methods" SW-846. Two characterist ics, react ivi ty and ignitability, are totally or partly prose definitions.

A. Ignitability

This characteristic identifies a solid was te as dangerous because

of its ability to create a fire hazard during storage, treatment

or disposal. Most ignitable wastes are liquids for which a

standard flash point test method is spelled out. Oxidizers,

ignitable compressed gases and solids may also create such hazards.

The latter have nOT or prose definitions.

1• Ignitable Liquids - The standard test measures the flash point

of liquid wastes that create a hazard because of their flammability. The Van Nostrand Reinhold Chemical Dictionary defines

flash point as "the temperature at which a liquid gives off a

vapor sufficient to form an ignitable mixture with the air

near the surface of the liquid or within the test vessel."

Waste liquids, such as gasoline, are classed as dangerous

wastes if their flash point is less than 140 0 F. using the

standard testing method.

The method specified in Appendix A-I uses a closed cup tester

to measure flash point. For purposes of this regulation, the

test liquid is introduced to a standard closed container

heated to 1400 F and an ignition source supplied. If the

test liquid flashes (ignites) the waste meets the characteristic of ignitability. (Method A - Flash/No Flash in Appendix

A, Attachment 1 should be used.)

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2.

.---.

Ignitable Solids - The test is described in Appendix A,

paragraph A2 and is a prose test.

_.J

3. Ignitable Compressed Gases - The test for ignitable

compressed gas first requires a prose definition for a

compressed gas and a referenced test method for liquids

having high vapor pressures. Unlike ignitable liquids,

candidate wastes are tested for flammability at room temperatures by opening a valve mixing with air, and applying

an ignition source. The method is given in Appendix A,

paragraph A3 and Attachment 2.

4. Oxidizers - The test ls described in Appendix A, paragraph

A4 and Attachment 3.

B. Corrosivity

The corrosivity characteristic is designed to identify wastes

which might pose a hazard to human health or the environment due

to their ability to:

1. Mobilize toxic metals if discharged into a landfill

environment;

2.

3.

Require handling, storage, transportation and management equipment to be fabricated of specially selected

material of construction; and

Destroy human or animal tissue in the event of inadvertant contact.

.-........--

C.

In order to identify such potentially hazardous materials, the

department has selected several properties upon which to base the

definition of a corrosive waste. These properties are pH and

corrosivity toward Type SAE 1020 steel. The pH of a waste mixture

is a measure of its acidic or basic properties, with a scale of 0

to 14. A strongly acidic mixture of sulfuric acid would have a pH

approaching zero whereas a strongly basic mixture like sodium

hydroxide may have a pH approaching 14. Pure water being neither

acidic or basic has a pH in the middle of the scale, or 7. The

corrosivity test is designed to detect wastes that would corrode

steel quickly. Appendix B presents methods for measuring the pH of

aqueous wastes and for determining whe~her the was~e is corrosive

to steel.

Reactivity

The regulation defines reactive wastes to include wastes which:

(1) readily undergo violent chemical change; (2) react violently

or form potentially explosive mixtures with water; (3) generate

toxic fumes when mixed with water or, in the case of cyanide or

sulfide bearing wastes, when exposed to mild acidic or basic conditions; (4) explode when subjected to a strong initiating force;

(5) explode at normal temperatures and pressures; or (6) fit within

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.---... .-,

.....>

D.

the Department of Transportation's forbidden explosives, Class A

explosives, or Class B explosives classifications•

This definition is intended to identify wastes which, because of

their extreme instability and tendency to react violently or

explode, pose a problem at all stages of the waste management

process. The definition in Appendix C is, to a large extent, a

paraphrase of the' narrative definition employed by the National

Fire Protection Association.

Extraction Procedure Toxicity

The Extraction Procedure (EP) is designed to simulate the leaching

a waste will undergo if disposed of in an improperly designed

sanitary landfill. It is a laboratory test in which arepresentative sample of a waste is extracted with distilled water maintained at pH = 5 using an acetic acid - sodium acetate buffer. The

extract obtained from the EP is then analyzed to determine if any

of the thresholds established for the eight elements (i.e., arsenic,

barium, cadmium, chromium~ lead, mercury, selenium, silver), four

pesticides (i.e., Endrin, Lindane, Methoxychlor, Toxaphene), and

two herbicides (i.e., 2,4,5-Trichlorophenoxypropionic acid,

2,4-Dichlorophenoxyacetic acid) have been exceeded. If the EP

extract contains anyone of the above substances in an amount

equal to or exceeding the levels specified in Chapter 173-303 WAC,

the waste possesses the characteristic of Extraction Procedure

Toxicity and is either an extremely hazardous or dangerous waste.

The Extraction Procedure which is detailed in Appendix D and

summarized in Figure 1 of Appendix D consists of 5 steps:

1. Separation Procedure

A waste containing unbound liquid is filtered and if the

solid phase is less than 0.5 percent of the waste, the

solid phase is'discarded and the filtrate analysed for

trace elements, pesticides, and herbicides (step 5). If

the waste contains more than 0.5 percent solids, the

solid phase is extracted and the liquid phase stored for

later use.

2. Structural Integrity Procedure/Particle Size Reduction

Prior to extraction, the solid material must either pass

through a 9.5 mm (0.375 in.) standard sieve, have a surface area per gram of waste of 3.1 cm2, or if it consists of a single piece, be subjected to the Structural

Integrity Procedure. The Structural Integrity Procedure

is used to demonstrate the ability of the waste to remain

intact after disposal. If the waste does not meet one of

these conditions it must be ground to pass the 9.5 mm sieve.

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••••• 0:

3.

4.

.-

Extraction of Solid Material

The solid material from step 2 is extracted for 24 hours

in an aqueous medium whose pH is maintained at 5, using

0.5 N acetic acid- sodium acetate buffer.

Final Separation of the Extraction from the Remaining

Solid

After extraction, the liquid:solid ratio is adjusted

to 20:1 and the mixture of solid and extraction liquid

are separated by filtration. The solid is discarded and

the liquid combined with the filtrate obtained in step 1.

This is the EP extract that is subjected to the evaluation requirements in WAC 173-303-090(8).

5. Testing Analysis of EP Extract

Inorganic and organic species are identified and quantified using the appropriate methods in Appendix D of this

manual.

III. Narrative of WDOE Tests for Criteria Covering Persistent Classes

of Chemical Compounds

Chapter 173-303 WAC identifies two classes of chemical compounds that

present a long term threat because they tend to persist, bioaccumulate

and present a chronic threat to human health and the environment. These

classes are halogenated hydrocarbons and polycyclic aromatic hydrocarbons.

To mimic the inherent nonwater solubility, and lipid (fat) solubility

of such compounds, the department uses a mild organic solvent, petroleum ether, followed by more specific analyses for each of the two

classes ,

It is important for the reader to understand that this procedure is

intentionally broad and inclusive rather than a compound-by-compound

analysis. As such, the petroleum ether solubility test should be

viewed as a screening test, which alerts the analyst to the presence of

potentially hazardous materials. At threshold concentrations of such

persistent materials, further analysis for the presence of genetically

active chemicals or the use of short-term bioassays Eor mutagenicity is

advised. The Department of Ecology, Hazardous Waste Section, should

be consulted before any such tests are undertaken.

A. Crude Sample Extraction for Halogenated and Polycyclic Aromatic

Hydrocarbon Analysis

Initial extraction procedures will depend upon the physical form

and mixtures of the crude sample. For example, the presence of

moisture in the sample will dictate the use of isopropyl alcohol/

petroleum ether extraction to dissolve water. Dry samples can be

-4-
extracted directly with petroleum ether. Peccoleum ether extracts

that are greater than 1 percent of the crude sample are then

subjected to the halogenated hydrocarbon and/or the polycyclic

aromatic hydrocarbon analyses detailed below.

Appendix E contains the specific procedures for crude sample

extraction.

B. Halogenated Hydrocarbon Analysis

The halogenated hydrocarbon procedure consists of combusting the

petroleum ether extract in a "Parr" bomb. This converts all

petroleum ether soluble organic compounds to more simple chemical

forms. qalogenated (i.e •• contains chlorine. fluorine. iodine or

bromine) compounds break down to form the respective ion forms

(i.e •• chlorides. fluorides. iodides and bromides). These are

water soluble. The Parr bomb residue is then rinsed with water and

the solution analyzed for the respective halide. Since the most

common halogen is chlorine. these procedures include a colorimetric test for the chloride ion in water. commonly used in water

quality analyses. Similar tests for the iodide. fluoride and

bromide ions are available upon request from the department and

taken from similar analytical sources. The Parr bomb and colorimetric test procedure for the chloride ion is described in

Appendix F.

When the analyst knows what particular halogenated compounds are

present. chromatographic methods may be used to determine threshold

concentrations. An example of such a method is described in· the

EPA method 612 for chlorinated hydrocarbons.

->,

. .

"--"

c. Polycyclic Aromatic Hydrocarbon Analysis

The polycyclic aromatic hydrocarbon analysis uses a series of

extractions to isolate polycyclic (many fused benzene rings)

compounds that are of interest because of their persistence.

bioaccumulation and chronic disease causing properties - the so

called neutral polycyclic compounds. The extractions and solvents

are designed to eliL~nate basic and acid groups as well as straight

chain and oxygenated groups attached to the fused benzene rings.

The procedures shown in Appendix G also allow the use of high

pressure chromatographic methods to further narrow the range of

neutral compounds to the 4-. 5-. and 6-ringed polycyclics. This

step is optional. For example. the analyst may show by chromatographic methods that a significant part of the extract is

napthalene. a 2-ringed compound. Such a result. when subtracted

from the solvent extraction result. may show a net residue of less

than one percent and therefore would not designate the waste by the

test method •

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APPENDIX

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APPENDIX A

CHARACTERISTIC OF IGNITABILITY REGULATION

A solid waste exhibits the characteristic of ignitability if a representative sample of the waste has any of the following properties:

AI. It is a liquid, other than an aqueous solution containing less

than 24 percent alcohol by volume, and has a flash point less than

600 C (1400F), as determined by a Pensky-Martens Closed Cup

Tester, using the test method specified in ASTM Standard D-93-79 or

D-93-BO, or a Setaflash Closed Cup Tester, using the test method

specified in ASTM standard D-327B-78. T~~t standard procedure is

attached to Appendix A, as Attachment 1. Method A, Flash/No Flash

should be used.

A2. It is not a liquid and is capable, under standard temperature and

pressure, of causing fire through friction, absorption of moisture

or spontaneous chemical changes and, when ignited, burns so

vigorously and persistently that it creates a hazard.

A3. It is an ignitable compressed gas as defined in 49 CFR 173.300 and

as determined by the test methods described in Attachment 2

of Appendix A.

A4. It is an oxidizer as defined in 49 CFR 173.151, which is provided as

Attachment 3 in Appendix A•

A-I
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APPENDIX A

Attachment 1

ASTM STANDARD D-93-79

ASTM STANDARD D-3278-78

ASTM STANDARD D-93-80

American Society for Testing and Materials Standards

are protected by copyright. Copies of ASTM standards

can be obtained by writing to the following address:

ASTM

1916 Race Street

Philadelphia, FA 19103

A-2
..'

...--.....

..·.1

APPENDIX A

Attachment 2

IGNITABLE COMPRESSED GAS

For the purpose of this regulation, the following terminology is defined:

1. Compressed gas. The term "compressed gas" shall designate any

material or mixture having in the container an absolute pressure

exceeding 40 p.s.i. at 700F or, regardless of the pressure at

70oF, having an absolute pressure exceeding 104 p.s.i. at 130oF,

or any liquid flammable material having a vapor pressure exceeding

40 p.s.i. absolute at 1000F as determined by ASTM Test D-323.

2. Ignitable compressed gas. Any compressed gas as defined in paragraph (1) of this section shall be classed as an "ignitable

compressed gas" if any one of the follOWing occurs:

a. Either a mixture of 13 percent or less (by volume) with air

forms a flammable mixture or the flammable range with air is

wider than 12 percent regardless of the lower limit. These

limits shall be determined at atmospheric temperature and

pressure. The method of sampling and test procedures shall

be acceptable to the u.S. Bureau of Explosives.

b. Using the U.S. Bureau of Explosives' Flame Projection Apparatus

(see Note 1), the flame projects more than 18 inches beyond

the ignition source with valve opened fully, or, the flame

flashes back and burns at the valve with any degree of valve

opening.

\

c. Using the U.S. Bureau of Explosives' Open Drum Apparatus (see

Note 1), there is any significant propagation of flame away

from the ignition source.

d. Using the U.S. Bureau of Explosives' Closed Drum Apparatus (see

Note 1), there is any explosion of the vapor-air mixture in

the drum.

NOTE 1: A description of the U.s. Bureau of Explosives' Flame Projection

Apparatus, Open Drum Apparatus, Closed Drum Apparatus, and method

of tests may be procured from the U.s. Bureau of Explosives.

A-3
,~,

APPENDIX A

Attachment 3

OXIDIZER

" 17:1.I.'>1 Oxid iz cr: defini! iun.

An o xidizvr for the purpose- uf lbi.s

suncnap u-r is a substance xuch a.:; :,

chtorat c. pc rruauganatc. inorgnntc p.-r

oxide, or a n it ratc. that yields oxva.-n

readily to stimulate the combustion of

oruanir matter,

(49 U,S.C, lMO:1. lMl'4, 1808: 49'CFR 1.53 l!l'd

App, A lo Parl 1)

lArndt. li:l-9-l, '\1 FIt 1601::1, Apr, If" 1!l7ti,

:l,i .uuendr-d by Amdl. 17;1-124, 4-l I-'H, :lIIG'I,

:\lar:ll. 1979J

R Ii:L!.'>1a Oq:ani.. perux id ..: d..fin it ion,

(a) An orn.uuc compound cont.a.ining

the uivalcut -0-- 0- structun- and

which may be considered a derivat.ive

'of h ydrouun peroxide where OlW or

mor« of the h ydrog eu atoms hav«

bCl:n r e p lacvd by on.:ani" rud ica ls must

be classed as an orgnuic peroxide

unless:

(1) The mut.r-ria l meets the dofin ilion of all c x plu-av c- A or exptosiv« II,

as prc,:cribeu ill Subpart C of t his part,

in which cas" it must bl' classed as an

e xploxiv«.

(2) Till' mat eri.u is Iorbiddun to OL'

orr·:red for t rruisport.auon uccorduu: u.

§ 17:!,101 or 1';:3,:!1 of this subchapter,

(3) It is dc-t crrntncd that the predorni n.uu, 1Iaz:,n1 uf t hc mnt crlnl CUlll:tillitl~ all urg'l-nit, pcrox ide is other

than that of all oruanic peroxide. or

(-1) Accordi iu; tll data on file with

t lu- Mnt crinlx Trunxuort nt ion Bureau,

it l::lS bee-n clct crnuricd i luu, th" m a t crial docs not pn's,'lIl a nazard ill t r.ms-

[HJrlatiull,

lAlI1ell. 1,3,.4,\, 4! f'n -lOGlH, Sept. 20, 1'1-;/j,

a:; :l:l~\'[lih'd h:. :\ll\dt. 11'3 Li~j. 45 Fit :i4';OJ.

!\1.l~ ~:.!. t BSu:

A-4
·---....

APPENDIX B

CHARACTERISTIC OF CORROSIVITY R8GULATION

A solid waste exhibits the ~aracteristic of corrosivity if a representative

sample of the waste has either of the following properties.

l.H. It is aqueous and has a pH less than or equal to 2 or greater than

or equal to 12.S, as determined by a pH meter using the test

method specified in the Attachment 1 to Appendix B.

B2. It is a liquid and cor~odes steel (SAE 1020) at a rate greater

than 6.3S mm (O.2S0 inch) per year at a test temperature of SsoC

(130°F) as determined by the test method specified in NACE

(National Association o~ Corrosion Engineers) Standard TM-01-69

and described in the Attachment 2 to Appendix B.

B-1
--

APPENDIX B

Attachment 1

pH MEASUREMENT

Scope and Application

This method* is applicable to aqueous wastes and those multiphasic wastes

where the aqueous phase comprises at least 20 percent of the total volume of

the waste.

Summary

The pH of the sample is determined e1ectrometrical1y using either a glass

electrode in combination with a reference potential or a combinqtion electrode. The measuring device is calibrated using a series of solutions of

known pH.

Interferences

1. The glass electrode, in general, is not subject to solution interferences from color, turbidity, colloidal matter, oxidants, reduct ants

or high salinity.

2. Sodium error at pH levels greater than 10 can be reduced or eliminated

by using a "low sodium error" electrode.

3. Coatings of oily material or particulate matter can impair electrode

response. These coatings can usually be removed by gentle wiping or

detergent washing, followed by distilled water rinsing. An additional

treatment with hydrochloric acid (1 + 9) may be necessary to remove any

remaining film.

4. Temperature effects on the electrometric determination of pH arise

from two sources. The first is caused by the change in electrode

output at various temperatures. This interference can be controlled

with instruments having temperature compensation or by calibrating the

electrode-instrument system at the temperature of the samples. The

second source is the change of pH inherent in the sample at various

temperatures. This error is sample dependent and cannot be controlled;

it should, therefore, be noted by reporting both the pH and temperature

at the time of ~na1ysis.

Apparatus

1. pH Meter-laboratory or field model. A wide variety of instruments

are commercially available with various specifications and optional

equipment.

*This method has been adapted from Method 150.1 of "Methods for the Analysis

,,-.' of Water and Wastewater," EPA-6000/4-79-020, U.S. EPA, Efo1SL, Cincinnati, OH

45268.

B-2
.,..............

2. Glass electrode.

0~" ... 3. Reference electrode a silver-silver chloride or other reference

electrode of constant potential may be used.

NOTE: Combination electrodes incorporati~g both measuring and referenced

functions are convenient to use and are available with solid, gel

type filling materials that require minimal maintenance.

4. Magnetic stirrer and Teflon-coated stirring bar.

5. Thermometer or temperature sensor for automatic compensation.

Reagents

1. Primary standard buffer salts are available from the National Bureau of

Standards and should be used in situations where extreme accuracy is

necessary. Preparation of reference solutions from these salts requires

some special precautions and handling 1/ such as low conductivity

dilution water, drying ovens, and carbon dioxide free purge gas. These

solutions should be replaced at least once each month.

2. Secondary standard buffers may be prepared from NBS salts or purchased

as a solution from commercial vendors. Use of these commercially

available solutions, that have been validated by comparison to NBS

standards, are recommended for routine use.

Calibration

1. Because of the wide variety of pH meters and accessories, detailed

operation procedures cannot be incorporated into this method. Each

analyst must be acquainted with the operation of each system and

familiar with all instrument functions. Special attention to care of

the electrodes. is recommended.

2. Each instrument/electrode system must be calibrated at a minimum of

two points that bracket the expected pH of the samples and are approximately three pH units or more apart. Various instrument designs may

involve use' of a "bal.a nc e " or "standardize" dial and/or slope adjustment as outlined in the manufacturer's instructions. Repeat adjustments

on successive portions of the two buffer solutions as outlined in

procedure 8.2 until readings are within 0.05 pH units of the buffer

solution value.

Procedure

1. Standardize the meter and electrode system as outlined in Section 7.

2. Place the sample or buffer solution in a clean glass beaker using a

sufficient volume to cover the sensing elements of the electrodes and

to give adequate clearance for the magnetic stirring bar. If field

'-/! 1/ National Bureau of Standards Special Publication 260.
' .. .....j

3.

4.

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. ,"

measurements are being made the electrodes may be immersed directly in

the sample stream to an adequate depth and nov ed in a manner to insure

sufficient sample movement across the electrode sensing element as

indicated by drift free «0.1 pH) readings.

If the sample temperature differs by more than 20 C from the buffer

solution, the measured pH values must be corrected. Instruments

are equipped with automatic or manual compensators that electronically adjust for temperature difference. ~efer to manufacturer's

instzuct t ons ,

After rinsing and gently wiping the electrodes, if necessary, immerse

them into the sample beaker or sample stream and stir at a constant

rate to provide homogeneity and suspension of solids. Rate of stirring

should minimize the air transfer rate at the air water interface of the

sample. Note and record sample pH and temperature. Repeat measurement

until values differ by less than 0.1 pH units.

Bibliography

1. Standard Methods for the Examination of Water and Wastewater, 14th

Edition, p , 460, (l97S).

2. Annual Book of ASTM Standards, Part 31, "Water," Standard D1293.

B-4
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APPENDIX B

ATTACHMENT 2

CORROSIVITY TOWARD STEEL

Introduction

This methodt is applicable to either aqu~ous or non aqueous

liquid wastes.

Summary of the Method

This test exposes coupons of SAE Type 1020 steel to the

liquid waste to be evaluated and, by measuring the degree to

which the coupon has been dissolved, determines the corrosivity

of the waste.

Precautions and Comments

1. In laboratory tests, such as this one, corrosion of

duplicate coupons is usually reproducible to within + 10%.

Occasional exceptions. in which large differences are

~bservedt can occur under conditions where the metal

surfaces become passivated. Therefore, at least duplicate determinations of corrosion rate should be made.

2. A circular specimen of about 3.75 em (1.5 inch) diameter

is a convenient shape for laboratory use. With a thickness of approximately 0.32 cm (0.125 inch) and a 0.80 cm

(0.4 inch) diameter hold for mounting, these specimens

will readily pass through a 45/50 ground glass joint of. a

distillation kettle. The total surface area of a circul&r

apeclmen is given by the following equation:

5.3-

(

tThis method i8 based on NACE Standard TM-Ol-69(1972 Revision),

-Laboratory Corrosion Te!ting ~f M~tal~ for thp Process Indu8trle

National Association of Corrosion Engineers, 3400 ~est Loop Sout~

Boust~n. TX 77021

B-5
C

,, . ....

,. . .

A • 3.14/2(D2_d2)+(t)(3.14)(D)+(t)(3.14)(d)

d • diameter of th~ mounting hole. If the hole is completely

.•.r where t • thickne ss, D • di aale t er of the specimen, and

..

covered by the mounting support, the last term (t){3.14)(d)]

1n the equation is omitted.

3. All coupons should be measured carefully ~o permit

accurate calculation of the exposed areas. An area calculation accurate to ! 1% is usually adequate.

4. More uniform results may be expected if a substantial

layer of metal is removed froa the coupons prior to testing

the corrosivity of the vste. This cen be accomplished

either by chemical treatment (pickling), electrolytic

removal, or by grinding with a coarse abrasive. At

1~ least 0.000254 cm (0.0001 inch) or 2 to 3 mg/cm2 should

be removed. Final surface treatment ~hould include

finishing with 1120 abrasive paper or cloth. Final

cleaning consists of scrubbing with bleachfree scouring

powder, followed by rinsing in distilled water, then

acetone or methanol, end finally air drying. After

final cleaning the coupon should be stored in a desieeator until used.

5 •.The minimum ratio of volume of waste to area of the

metal eoupon to be used in this test is 40 ml/cm2•

EquIpment

1. A versatile and convenient apparatus should be ~sed, con-

'''\-,

V'

stating of a kettle or flask of suitable size (usually 500

to 5000 .Illilietars), a ~eflex condenser with atmospheric

Zit'll-: '''N- 'OWO"'Ol .. 1:d f4("1 ,y,.. ..!)]ti

J.~... ' • .J .11..' Joe,Je

L8. - g IId't B-~
.-,

• Beal. a thermowell and temperature regulating device , a

heating device (mantle, hot plate, or bath), and a specimen

s.3-3 I

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Re~~sioD A 8/8/80

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...

Bupport system. A typical resin flask set up for this type

test 1s shown in figure 1.

2. The supporting device and container should not be

affected by or cause contamination of the waste under test.

3. The method of supporting the coupons will vary with

the apparatus used for conducting the test but should be

designed to insulate the coupons from each other physically

and ~l~ctrically and to insulate the coupons from any metallic

container or other device used in the test. Some common

support materials include: glass, fluorocarbon or coated metal.

4. The shape and form of the coupon support should assure free

contact with the waste.

Test Procedure

1. Assemble the test apparatus as described the "Equipment"

section above.

2. Fill the container with the appropriate amount of waste.

(See IS under the ·Precautions and Comments" section.)

3. Begin agitation at a rate sufficient to insure that

the liquid is kept well mixed and homogeneous.

4. Using the heating device bring the temperature of

~be waste to 55° C (130° F).

s. If the anticipated corrosion rate 1s moderate (i.e.,

<.254 mmpy)., the test should be run for at leat 200 hours to

insure adequate weight 108S to permit accur.te results to be

( obtained. If the corrosion rate 1. low (1.e., <.0254 mmpy)·.,

B-7

• Change II

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then the teat duration should be on the order of 2000 houre.

In caaes where the anticip~ted corrosion rate 1s completely

unKnown, initial testing should be performed using a 200

hour duration.

6. In order to accurately determine the amount of material

lost to corrosion, the coupons have to be cleaned after

immersion and prior to weighing. The cleaning procedure

should remove all products of corrosion while removing a

minimum of Bound metal. Cleaning methods can be divided

into three general categories:

electrolytic.

mechanical, chemical and

Mechanical cl~aning includes scrubbing, scraping, brushing

and mild abrasive is the most popular of these methods; the

and ultrasonic procedures. Scrubbing with a bristle brush

c

others are used in cases of heavy corrosion as a first step

in removing heavily encrusted corrosion products prior to

scrubbing. Care should be taken to avoid removing sound metal.

Chemical cleaning implies the removal of material from

the surface of the coupon by dissolution In an appropriate

~olvent. Solvents such as acetone, dichloromethane, and

alcohol are used to remove 011, grease or resinous materials,

and are used prior to immersion to remove the products of corrosion.

Solutions suitable for removing corrQsion from the steel

coupon are:

......

. . i

"-.../ - Solution

_ 20% NaOR + 200g/1 zinc dust

or

Soaking Time

5 min

Temperature

Beriling

(

B-8

Conc. BCI + SOg/1. SnC12 + 20r.'1 Sr.-'3 !'r.til clean Cold
,~. -- .

,

Electrolytic cleaning should be preceeded by scrubbing

to reaove loosely adhering corrosion products. One method of

electrolytic cleaning that can be employed is:

Solution

Anode

Cathode

Cathode current density

Inhibitor

Teaperature

Expo8ure Period

Carbon"or lead

Steel coupon

20 amp/cm 2 (129 amp/in 2)

2 cc organic inhibitor/liter.

74·C (165°F)

3 minutes

Rote: Precautions must be taken to insure good electrical

:;7'. .

~~contact vith the coupon, to avoid 'contamination of the c Le a n Ln g

.olution vith easily reducible metal 10ns, and to insure

that inbi~itor decomposition has not occurred. Instead of

( ..

using a proprietary inhibitor, 0.5 gIl or either'diorthotolyl

thiourea or qulnolin etblodide can be used.

Vhatever treatment is employed to clean the coupons,·its

effect in removing sound metal ahould be determined using

blank (i.e., a coupon that has not been exposed to the waste).

The blank should be cleaned along with the test coupon and

it. va.te loss subtracted from that calculated for the test

coupon ••

7. After corroded specimens have been cleaned snd dried.

they are reveiahed. The veight los. is employed a8 the

principal measure of corrosion. Use of weight 10s8 a8 8

B-9
I 5.3-6

__'N

1ev18lon A 8/8/80

- - -~ '-_..._.~-.-.-.:'"~---"'_~--_"".~--- ...._..:_-_._----_ .. -

:mea8ure of corr08lon required making the assumption that

all .e~ght 1088 has been due to generalized corrosion

and Dot localized pittiug. In order to determine the

eorrosiou Tate for purpose of this requlation, the following

foraula i8 used:

Corrosion late (mmpy) - (weiRht loss) (11.lAS)·

(area) (time)

where weight 10s8 is in milligrams, area 1n square

centimeters, time in hours, and corrosion rate in

mi11imters per year (mmpy).

c

.. '""~

* Change '3 B-10
,..-..-.

APPENDIX C

CHARACTERISTIC OF REACTIVITY

A solid waste exhibits the characteristic of reactivity if a representative

sample of the waste has any of the following properties:

Cl. It is normally unstable and readily undergoes violent change

without detonating.

C2. It reacts violently with water.

C3. It forms potentially explosive mixtures with water.

C4. When mixed with water, it generates toxic gases, vapors or fumes

in a quantity sufficient to present a danger to human health or .

the envi ronment .

C5. It is a cyanide or sulfide bearing waste which when exposed to

pH conditions between 2 and 12.5, can generate toxic gases, vapors

or fumes in a quantity sufficient to present a danger to human

health or the environment.

C6. It is capable of detonation or explosive reaction if it is subjected to a stong initiating source or if heated under confinement.

C7. It is readily capable of detonation or explosive decomposition or

reaction at. standard temperature and pressure. See the Attachment 1 to Appendix C for further definition of explosive materials.

C8. It is a forbidden explosive as defined in 49 CFR 173.51, or a

Class A explosive as defined in 49 CFR 173.53 or a Class B explosive as defined in 49 CFR 173.88. See Attachment 2 of Appendix C.

C-l
·..--.....

APPENDIX C

ATTACHMENT 1

DEFINITION or E~PLOSIVE MATERIALS

For purposes of this regulation a waste which is a

reactive waste by reason of explos1vity is one which meets

one or more of the following descriptions:

. 1. Is explosive and ignites spontaneously or undergoes

marked decomposition when subjected for 48 consecutive

h~urs to a temperature of 75°C (167°F).

2. Firecrackers, flash crackers, salutes, or similar

commercial devices which produce or are intended to

produce an audible effect, the explosive content of

which exceeds 12 grains each in weight, and pest control

bombs, the explosive content of which exceeds lR grains

each.in weight; and any such devices, without respect

to explosive content, which on functioning are liable

to project or disperse metal, glass or brittle plastic

fragments.

3. Fireworks that combine an explosive and a detonator

or blasting cap.

4. Fireworks containing an ammonium salt and a chlorate.

5. Fireworks containing yellow or white phosphorus~

6. Fireworks or fireworks compositions that ignite

spontaneously or undergo marked decomposition when

subjected for 48 consecutive hours to a temperature of

75°C (167°F).

7. Toy torpedoes, the maximum outside dimension of

which exceeds 7/8 inch, or toy torpedoes containing a

mixture of potassium chlorate, black antimony and sulfur

with an average weight of explosive composition in each

torpedo exceeding four grains.

8. Toy torpedoes containing a cap composed of a mixture

of red phosphorus and potassium chlorate exceeding an

average of one-half (0.5) grain per cap.

9. Fireworks containing copper sulfate and a chlorate.

10. Solid materials which can be caused to deflagrate

by contact with sparks or flame Buch as produced by safety

fuse or an electric squib, but cannot be detonated (see Note

1) by means of a No.8 test blasting cap (see Note 2).

Example: Black powder and low explosives. c

C-2

(
(

(

(

11. Solid materials which contain a liquid ingredient,

and which, when uncon:ined (see Note 3), can be detonated

by m~an8 of a No.8 test blasting cap (see Note 2); or

which can be exploded in at least 50 percent of the

trials in the Bureau of Explosives' Impact Apparatus

(see Note 4) under a drop of 4 inches or more, but cannot

be exploded in more than 50 percent of the trials under

a drop of less than 4 inches Example: High explosives,

commercial dynamite containing a liquid explosive ingredient.

12. Solid materials which contain no liquid ingredient

and which can be deto~ated~ when unconfined (see Note 3),

by means of No.8 test blasting cap (see Note 2)j or

which can be exploded in at least 50 percent of the

trials in the Rureau of Explosives' Impact Apparatus

(see Note 4) under a drop of 4 inches or more, but cannot

be exploded 1n more than 50 percent of the trials under

a drop of less than 4 inches. Example: High explosives,

commercial dynamite containing no liquid explosive ingredient, trinitrotoluene, amatol, tetryl, picric acid,

ureanitrate, pentolite, commercial boosters.

13. Solid materials which can be caused to detonate

when unconfined (see Note 3), by contact with sparks or

flame such as produced by safety fuse or an electric

squib; or which can be exploded in the Bureau of Expl~sives'

Impact Apparatus (see Note 4), in more than 50 percent

of the trials under a drop of less than 4 inches. Example:

Initiating and priming explosives, lead azide, fulminate

of mercury, high explosives.

14. Liquids which may be detonated separately or when

absorbed in sterile absorbent cotton, by a No.8 test

blasting cap (see Note 2)j but which cannot be exploded

in the Bureau of Explosives' Impact Apparatus (see Note

4), by a drop of less than 10 inches. The liquid must

not be significantly more volatile than nitroglycerine

and must not freeze at temperatures above minus 10°F.

Example: High explosives, desensitized nitroglycerine.

15. Liquids that can be exploded in the Bureau of

Explosives' Impact Apparatus (see Note 4) under a drop

of less than 10 inches. Example: Nitroglycerine.

16. Blasting caps. These are small tubes, usually

made of an alloy of either copper or aluminum, or of

molded plastic closed at one end and loaded with a charge

of initiating or priming explosives. Blasting caps (see

Note 5) which have been provided with a means for firing

by an electric current, and sealed, are kr0~~ a~ electric

blasting caps.

C-3
17. Detonating primers which contain a detonator and an

additional charge of explosives. all assembled in a suitable envelope •.

18. Detonating fuses. which are used in the military

Bervice to ·detonate the high explosive bursting charges

of projectiles. mines. bombs. torpedoes, and grenades.

In addition to a powerful detonator. they may contain

Beveral ounces of a high explosive. such as tetryl or

dry nitrocellulose, all assembled in a heavy steel envelope. They may also contain a small amount of radioactive

component. Those that will not cause functioning of

other fuses, explosives, or explosive devices in the

same or adjacent containers are classed as class C explosives and are not reactive waste.

19. A shaped charge. consisting of a plastic. paper. or

other suitable container comprising a charge of not to

exceed 8 ounces of a high explosive containing no liquid

explosive ingredient and with a hollowed-out portion

(cavity) lined with a rigid material.

20. Ammunition or explosive projectiles. either fixed.

semi-fixed or separate components which are made for use

In cannon. mortar. howitzer. recoilless rifle. rocket.

or other launching device with a caliber of 20 mm or

larger.

21. Grenades. Grenades. hand or rifle. are small metal

or other containers designed to be thrown by hand or projected from a rifle. They are filled with an explosive

or a liquid. gas. or solid material such as a tear ga9

or an incendiary or smoke producing material and a bursting

charge.

22. Explosive bombs. Explosive bombs are metal or

other containers filled with explosives. They are used in

warfare and include airplane bombs and depth bombs.

23. Explosive mines. Explosive mines are metal or composition containers filled with a high explosive.

24. Explosive torpedoes. Explosive torpedoes, such as

those used in warfare. are metal devices containing a means

of propulsion and a quantity of high explosives.

(

~.

25. Rocket ammunition •.Rocket ammunition (including

guided missiles) is ammunition designed for launching from

a tube, launcher, ra~16, trough, or other launching deVice.

in which the prope116~: ~~terial is a Bc}1d propellant

explosive. It consists of an igniter, rocket motor. and

projectile (warhead) either fused or unfused. containing

high explosives or chemicals.

C-4
co

c.-

(

-.

26. Chemical ammunition. Chemical ammunition used in

warfare is all kinds of explosive chemical projectiles,

shells, bombs, grenades, etc., loaded with tear, or

other gas, smoke or incendiary agent, also such miscellaneous apparatus as cloud-gas cylinders, smoke generators,

etc., that may by utilized to project chemicals.

27. Boosters, bursters, and supplementary charges.

Boosters and supplementary charges consist of a casing

containing a high explosive and are used to increase the

intensity of explosion of the detonator of a detonating fuse.

Bursters consist of a casing containing a high explosive and

are used to rupture a projectile or bomb to permit release

of its contents.

28. Jet thrust units or other rocket motors containing a

mixture of chemicals capable of burning rapidly and produ~­

lng considerable pressure.

29. Propellant mixtures (i.e, and chemical mixtures

which are designed to function by rapid combustion with

little or no smoke).

~ote 1: The detonation test is· performed by placing ~he

sample in an open-end fiber tube which is set on the end

of a lead block approximately I 1/2 inches in diameter

and 4 inches high which, in turn, is placed on a solid

base. A steel plate may be placed between the fiber

tube and the lead block.

Note'2: A No.8 test blasting cap is one containing two

grams of a mixture of 80 percent mercury fulminate and 20

percent potassium chlorate, or a cap of equivalent strength.

Note 3: ·Unconfined" as used 1n this section does not

exclude the use of a paper or soft fiber tube wrapping to

facilitate tests.

Rote 4: The Bureau of Explosives' Impact Apparatus is a

testing device designed so that a guided 8-pound weight

may be dropped from predetermined heights so as to impact

specific quantities of liquid or solid materials under

fixed conditions. Detailed prints may be obtained from

the Bure~u of Explosives, 2 Pennsylvsnia Plaza, New York,

.Rew York, 10001.

Note 5: Blasting caps, blasting caps with safety fuse,

or electric blasting caps in quantities of 1,000 or

less are classified as class 0 explosives and not subject

to regulation as a reactive waste.

c-s
...--....,

APPENDIX C

ATTACHMENT 2

I ~:l.;ll F()rhidd.~n expl,,,iws.

Unless otherwise preJ\'idrd in t.h is

subrhapt.cr. the tnll1sporta l ion of t lH'

f o llowiu g c x ptosivcs ,s Ior ni ddc n:

(n.) Explosive compounds. mixtures

or devices which ignite .-;pon(:uwously

or undergo rna r k r d dr-com postt.iou

when su bjectr-d to a \C'lnjWratllf(' of

167" F. (7.')' C.) for 41\ consr-cu t iv.

hours.

(b) New explosive compounds, mixtures or devices except a.~ provided tor

in § 173,86,

(c) Explosive m i x t u rr-s or devir-cs

containing an arnrnorrium salt. nnd :1

chlorate.

<d) Ex nlosive mix! ures or r!P\"ic,'"

coritai nlug an acidic mr-t al sa.lt and :t

ch lorrur-.

(e) Leaking or durnrun-d packag.'s 1)[

explosives,

(f) Nit.roz lvr-e r in. rli,·th.\'\f'IH' t:I~'(',,1

din itrn.tc or ot lu-r li(l'lid n;lliosin's Ilnl

authorized hy H7,l,S:H"j or t h i. (Fl'r

shipmr-n t by motor vr-h ir-lr- ot h.-r Ilt;\:\

by common cnr r iur, :;",,' 177,8::2( lJ \ n r

this su br hap t.r-r.j

(g) Loadr-d fi rearms.

(h) Fireworks t.hn t ('o:nbilll' an ('Xplosivr- and a dr-t onn r or or h\a!:tilll\

cap,

(i) Piruworks con t n intru: yel\()\\' or

wh itc nhosnhorous.

(j) Toy torpedoes. \ he maximum Ollt·

sick dirru-nsion of wh ir-h pxcp.'ds ; •.

inch, or t.oy I.orp'.'d.,(,s co ut ai nuu; a.

mix! lin' of pot nsxiu rn ("lliorn! 1', l)1:l('K.

antimony, and su l I ur wu l: all al·cra!.:\,

\\,pigllt of l'xplll"h, "'lInDosil io u ill

each t orpvr!o {'xc{'l'din~: four f{rain:.:.

C-6
~'\

.... -. ,,~

~~

,,_.~ ..

11173.53 n,~finitinn of class ,\ explnsivcs.

(a) Type 1. Solid c xnloslvcs whicb

can be caused to ddla"rale by contact

with sparks or flame s;wh as producr-d

by safety fuse or an cu-ct.ric squib, hut

cannot be detonated (:;pc Notc 1\ bv

means of a No.8 test blast.i ng cap (.'iee

Note 2). Example: Black powder and

low explosives.

(b) Tvpc 2. Solid c x plostvcs which

contain a liquid explosive ingredient.

and which. whr-n unconfined i scc NOll"

3). can be dctol1:1.teo by means 0 f a No.

B ~~t blast ing cap (scc Note 2): or

which can be exploded in at least 50

percent of the t.rials in the Bureau of

Explosives' Impact Apparatus ':;t'l'

Note 4) i.nder :« drop of 4 inches or

more. but. cann«t be e x p ioded in rno rrthan 50 percent of ! he trials under a

drop of less than 4 inches. Example:

High explosives. commercial dynamite

containing a liquid explosive ing redient.

(c) Type 3. Solid explosives which

cont.ain no liquid explosive ingredient

and which can be detonated. when unconfined (see Note 3), by means of a

No.8 test blasting cap (s,'e Note 2): or

which can be exploded in at least 50

percent of the trials in the Bureau of

Explosives' Impact Apparutus (set'

Note 4) under a drop of 4 inches or

more, but cannot be exploded in mort'

than 50 percent of tl ie trials under a

drop of less than 4 inches. Example:

High explosives, cornuu-rciat dynamite

cont airiing no liquid explosive ingredient, trinitrotoluene, amatol. tctryt.

picric acid, urea nitrate. pcruolite. and

commercial boosters,

(d) Type 4, Solid cx plostvc-s which

can be caused to uet onate when unconfined (see Note 3). by contact .vith

sparks or flame such as nroducr-d by

safvt y lust' or .ui ell'l'lric squib: or

which can be exploded in the Bureau

of Explosives' Impact Apparatus (sec

Note 4), in more than 50 percent of

the trials under a drop, of lrss than -l

indies. Example: Initiating anti primin~ explosives. kad a;~idl'. Iu lm mat c of

mercury, et.c., u ud hi~h «xplosivvs.

ie) Type 5. l)t-s('nsil :'·.,·d liquid e x p lo-

:;i\'t'S are expl"s:\'t:,; wh icl: rna y bt' de tunated scparutrl y or \\'I1I'n :tbsorl)l·d in

suril« allSllr~)L'llt covt cn. by a No.

tl'st blast.Jng C:lP (,;,.,' l'\ul" I: b'UI

1\ idcll l.':lllnlJt l)t· ,'xplcdcd d! LllL'

. illlrl':lU lJf F":xplus!,'I'''; Impact AlJ:Jara·

tlH (SCI' Not.: 4). b.... a drop of kss than

\1) illCIl<·s. '1'1:" d,· .'·11....,1it"'!' II\Ust Iltll

iJ,; signil it'a:1L1:; I!:OI'\~ ','OI:Hile than 11i·

'lu~'ly(·prin,· :llld III.' d'·S(·11Sitiz,.-d 1'.'-

plush',' lIIust 111.1 fr'T/.I· a!. I(':II!JI'!','l'

lure,., above mlWl.~ Ill' I,'. E~:amp!e:

lIi~h l'xplosivl's. d"Sl'llsitiz.eu llitro~lYj't'rilH',

(f j 'I'vpe 6. Liquid explosi\"'s th:ll can

IJ<' "xplotlcd ill UIt· Burt'au of ExpLl-

:.IIt·S· 11lIpact Apparalus ISt'l' Noll' -li

under a drop of It's,,; than II) indl,·s.

Exarnp!«: ~;:tro~lycc:·;r:. Set:

1-;:l.S h:lJdl. i

. g: 'l':/I)C ~. }\I"l itlil:a l ;::~~ ~:t··. :\'" i.'-) a

rm-t al or p laxt.ic casiru, c:.>nl:lil:;:.;.; init ia t nu.. or pr:nlillf,: ('Xp!usi';es. ('::l.~S :\ ..

1'YPI' -t. l'IUll'r wit l: or \I'd ::u\i'. othcr

c x plosivcs. It is al'tiL':tll'd by .u:v cne

of several rnt'~1I1S, illl'luding a:1 l·!-'clri·

ca l pu lx«, it flanlt·. a s nock or de t o nat ion wa \'t', rnechanical impart (percussion) pr;'ssuriz"d ga.s. or lIigll .nr enstt.y

ligllt Iwam. It proudc,'S an ,'x;)]osive

output that. may be used to initiate anot hcr explosive or to perform work. A

time delay may be im-orpora n-d i n t.he

means of applying the st irnulus. or in

the initialing device- itself'.

(1) A di-t on.u ur (se(' Not." .1) is all initiating di-vico vot her than on,' prop...rIy describ,'(\ :1..~ a dct o n.u :!Or: fuze)

whic h contains no more Ulan 10 ~:r:(/l1:;

of total e xplosivcs weigl)~.•'xcilldin~

i~nition and de lay charues prr unit.

Tllere are different kind...; of detonators including the Iol lowing ;

Ii) Blasting- caps which :L~l' .u-t.lvat.cd

by safety ruse.

(ii) BI;1..-;till" caps wn ict: art' pe rcussion activa ted.

(iii) Blast ing caps which arc act.ivatI'd by rkxiule dctlln:Lt!Il~: V'J: d. iurludill~ .-

(:\) Delay connect or.. in p last.ic

slll'",llS which consist of ~l plastic

skL'\'e that. contains a suit.able delay

syxt cn: will) n'('('ptnr and .tor.or e x plostvc char~('s in till' ("'Iller portion.

l~adl l'lId Ill' I he s h-cvc I.; l::ack so that

fli-x ib le d.·tflllaling curd (';t:l be insertt'd lille) und Iockr-d to t:I<.· ('I,nll,'ctor:

I 131 Dela v conneci.orx ,:1 ;:;'.': :11 tubes

\\'}1i<'!1 ('uII.'-iisl of a Systl'lll .... i: I: a rvceu1.01' alld douor ehargt.' pU.>1lHd\t·d bl:-

l\\'l'\'n lv.,'u dt'l\Ina:..urs \I,:i~:~ I ~." t_'ntirf'

,1..··s,·llllJl:: pla"(:d ill 't :::<.t;,; IUUC

)la\'ill~ botll ('nds ",)(::1 :"):' ~h.~ inser·

t iUll of fl"xihl" ,flot..."I:L! :ll~ cord:

1\'1 l.Jl'!ay (·IIlllll·,·tlll':; ·.':lll ddona!-

~nt-~ \ord pi~~l~il:-) \\.-hlVi: r:on.:is! of (!t~l:lY

,'UJ:l.t:ct()rs :l.' 1!t'",-ribl.'<1 ::! ;';lr:lgraplI

\I::' I ,liii 'lll) 01 llli:; S"l'iIU!, til"l 1m",:

,:h,',rt It'ni<hts uf uetOI1,,'ill~ l'ord in·

sl'l'l"d into l.Jntll ':l1t1.~ alld crilIlp(.'d in

pL:.·,,; and

,.1): NOI1l'I"ctril' illS:·.;'III;,r;r·'lIlS and

L!,,!:(y 1';1 iJ:, whll'il COlhisl of blasting

..ap:; 10 which is a.'isl·mbll'd a ll'ngth of

dl'lonating ,oro tllaL :11:1)' have a

C-7
§ 173.53

t ransfr-r c xploslv« cbar;~r :1, :111' api"),

siti' .:nd,

(i\'! BI.;,')tinv, C:1l)S wllir'!l arc ac: i\':I:'

cd by gas pressu rizat ion 0, r enr-t.io n.

( v ) Bla,stil1f; c,ap:; wh irl: ar«: :lei i',"I.:I'<!

by a shock tube,

(vi) Elcrt r ic b last.i nz cap" ',I'~ljl'll a rractivated bv all electric' curront.

(2) A detonating primer (Sf'(' NOI" til

is an initiation n('vice for commcrrinl

use which cont ains more t.h a n 10

grams of total explosives we in ht , ex,

eluding ignition and dr-lay chan:":; 11fT

unit. '

(3) Dctonat.tnrr fuzes, class A, an'

used in till' military sr-rvlco to dr-t onate the high explosive bu rst.iru:

chnrues of projectiles, mines. bombs.

torpr-doos. and grenades, In addlt ion

to a powerful detonator, they may

contain several ounces of a hi~h e xplosive. such as tctryl or dry rut.roco l lulose. all assembled in It heavy steel I'llvelope. They may also contain a sm:1.11

amount of radioactive cornporu-nt.

Those that are so made and packr-d

that t h ey will not cause functioning of

other fuzes, cx ploxives, or I'xplo,o.;i\·"

devices in the same or adjacent con,

tainers are classed as class C explosives.

(h) Type 8_ Anv solid or liquid com,

pound: mlxt ure or df'vi('(' which is not.

specifically included in any of t.lw

above tvpos. arid wh irh under sPN'ia]

conditions may 1)1' 50 desir:n:u I'd :'Inri

examined by the BU;l':l.1I of Explosivc.s

and approved by t.h e Associate Director for OF;. Example: Sha[w ch:1.q~rs,

commercial.

(I) A shaped Cll:l.rge, eomnwrei.1.!.

consist:; of a pla:;tic, p:l.PN, or olll('r

suitable container comprising a chargr

of not to C'xf'('c:d 8 ouncps of :l. hir:h f'X'

plosivt' containing no lir;uid ('xplosh'"

ingredient and with a holl<>wp(J-Oll,

portion (ca\'ity> liri"d with a rigid m:l'

I.e;ial. DNo:lnl:jrs or other iniliarin~

elements may /lOt. he a.<;sembled in t h ....

c!c\'ice IInkss examilwu b~' til(' I1urf'au

of Explosi\'es :l.nd aPPrrl\,('u br llll' A,ssocin.tc Dircc!or for OF.,

(j) Alilmunition tor r(lllnOn, I\mmll'

nltion for cannon is fixed, sl'mi,fixcd

or sC'paratf' loading ammunition whi('h

is fir....d from :l. C:1./lnon, 1110rt:'lr, t.:lln,

howitzer or rpcoilks5 rifle,

(j) Ammunition for cunnO'l :ri/il

projeclill's, Amn1llnit ion, for r:'l nllO:1

Titl» 49--Transportation

',\'i::l cx plosivc projf'('t i lr«, "::1" :'rq.if""

i 1}' .:. ~n1()kp ;)roj(~(': iit s., ~tll·i'ndi:l.r::

;)r"~'('r'l i l ex. ;ilurllin:lt iri-; ;1n\:t:'('! il,·s. rl"

Shl-:~ i~, flxc,et aru rn u n i'{ot: :t:~:";I'!1,hl"d in

:1 :lldl ('IJl1s::;1it u: of till' ,'ar: ~,dL',l' COL',"~

('11!ll.,illing- Ille propl':lil~C: r!larlU' arod

priuu-r, al1n i 11l' p ro ii-r-: i;' " n;' .l i-vl l .

(1.1·,',1'<1 or unrLl;'~,t'd. !), It':,:: 1~~~ rll~,l·:":.

lr:l{'cr fUZflS, ex;,iu,;i ..(' -r :::1'1;: inn dt.'·

\"r,':_, or f\l7.I' I'arts \\ it l: "~:pirl,'i'.'I's

('()I1T:1int'd fh(';'t'in ln~.:; IJ1~ 1,., a.~:,i'n\·

hiI'd :n ammunition or inr"I:(ic'r! :n t.IIp

S:U;1I' flutsidc p:1rk:1l'," 1111'",:, :Ilipp,'d

h,\' or for the Dcpa 1'1mr II r. ')r D,,[ense

(POD' and in accordance wi t h r-st nbli::!ll'd pr:l"1 jet'S and I'r\H't'dlll'ls sp",'i,

fi('(1 hy DOD,

'.k) Er nl osir» nroicctilrs. F>;pl"":I'"

prn.i!'ctilf's arc sIll' II::, project,lt's, WOU'-

ilC·:l.d:;, or rock r-!. hrarl~, !na,j.-d wit l: rxnloi.ivr-s or hurst iru; rll~r..:-,'s, wu I: or

wit nout ot I1I'r n):1I,'~ial.., r"r lIS" in

cannons, gllns, t ubcs. 111::1': a r.: or O( II"r

firing or launching dr-virr:'.

,. J) Grcu ad cs. Gn'l1arft's, hanel or

ri Ile, arc small metal or ot hr-r containr rs dcsirmed I () be t IHo'.':11 h~: hand or

pnJj('cl.cd from a rifle, Til,')' :l.J'(~ fill ..d

with an e xp losivr- or a. liquid. ga.." or

xo l id matcrtat surh :'IS :l. t o x ic or tP:'IT

r::lS or an inr-cndiarv or :'l11ok,' p rorluciflr:; rnatcrial and a bu r:« int: rh:ln.(f',

\o\'hl'l1 shipPf'd wit 1l0\1! ,'\p!,-:;j','I'" or

bursting- rh:l.rl;PS, Sl''' ~~ l'i~,lOO(YI,

173:130, 173,:150, and 17~,:lB5,

(111) Erntos; 1'1' bombs. Ex nlosivc

bornhs arc 1I11'tai or other coni n iners

f:l~"<! \\'jl.h c x p lostvr-s. Th":: :'.l"l' u.""d in

w:1rh.rt' a.nd inr-Iudr- ~1'~{1:,lal1(' hombs

:t11<.1 Iil-pt h bnlllbs.

(11' F.,rp/osll'l' lIli7lr,~. E:,:plosi,,'l' mint'S

;HI' metal or eOl11posit ''.l''l <':0111 aincrs

filled wit 11 :l high explo:,i':[',

In, "~:::p/()":II'" lorprl!n,.I, F.xplnsirr

: "I'p..dof's, :"\ICI: :1.$ are user! i:l 'J:;trfare,

:\t',' 11)('( al c!,,\'irps conI aj:lil~l: :l. nW:1I1S

of prollulsion and a (;':a:::. ,I y q!' hid1

":-; ~)l o.,j':cs.

'p, [{oekel (1'71111111:11'(," 1\ ',C;:,I'I a 111 ,

1;l\II1:lion (inr:luding 1:'IHjl'd :11 i..;siIr,:"I is

:l.1~lJl1lll1itiQn c!f'sil:nNl f(lr Jallnr'llillg

Ir(:m :t tube, i:l.lIrH'IH'r. 1';1;1:" i rouG!1. or

nth"r In,lll1rllillfr dp\·:,'r, ill I,rhicll th~

;lr"p..Ilant mnlpri:1.1 is a solid prop!'l-

!a::1 pxplosi ..,c. II consists of :1.n iJ,(nitrr,

nwkd l11otor, :1.llr! projl'l'\ iJoo '\\':1.rht':1.dl

,'i: 11!'r fuz,'d or unfu;',I'<I, conl"ininghi;;!1 "~:plosi':r's or C'h':~1:r:"I''';, ·Rnrkpl.

:ull::1ilnil ion may 1)(' slIip;lf'd ('omplp(eC-8
.,~~.

. ,

Chapter I-,hsearch and Special Programs AJmini~tration 173.53

. ~-":' .~

. ". ;

""-"'

ly assembled or rnu y be shipr"J u n.issembled in one outxid« com.a im-r.

tq) A III IlL 101 u to i, .Ivf SIHu!l arIHs IL'iUt

exulosi ue prOj('t'ill.-s (II" i-ice n d i a rv p roiectiles. Ammunit ion for slllall arms

with explosive projvctiles and ammunition for small arms with inccndiary

projectilr-s is Ii xcd ammuniLion of caliber 20 mill imet us to be us-d in machine guns or c.umuns. and consists of

a metallic can ridge case, Llll' urimc r

and the propelling ctiargu. with e x p losive projectile or inccnd iary proivc t ile

with or without dc-tonnt.ing ftlzP: t lw

component parts necessarv for one

firing being all in one assernb ly. Detonating fuzes. t rncc-r Iuzr-s. explosive or

ignition devices or fuze parts wiLh explosives contained t hercrn 111ust not beassembled in anuuunit iou or included

in the same outside \.>ackag" unless

shipped by. for or to tile Dcpnrtrru-nts

of tile Army. Navy. and Air Force vI'

the U.S, Government or unless of a . type approved by the Department.

(1') Ctiem ical UIHIHlllliliolt. Chemical

ammunition uxcd in warfare is all

kinds of explm:iI.,. clu-nucal proj,·t:til,'s,

shells. born us, J.(l'l'lIac!<'s, ctc., load,'l\

with toxic, t ear. 01' o t h c r gas. smoke or

incendiary aJ.('·l\t, abo such m iscc llaneous apparatus as cloud-g as r-yl iudel'S. smoke gt'l\t'rat.ors, vt.c.. ui.u may

be utilized to proj,'ct cncmicals.

ls) Booste rs. h u rst crs, a.tid s u p plc- meula ru dill ro.:«. IlU(I:il"rs ;ulll SllPP]{'-

rncnt.uy ,:lIart'v:; '''')llsi~;t. uf :\ casing

COl\taining " Ill~~ll ,'xplosiv,' and arl'

used to incn·i\st' th,~ illll'nsi!.y oC ,'xpl\lsiun of th,~ dc-Iullator of a detonatillg

fuze. BlIrstt~rs consisl of a casing <.'0:1-

laining a IIigh I'xl_l\osin.' alld arc uSt'd

to rllptllr,· a IJl'llj'.·... ' ilt' \11' LJ\llllu tu

pl'l'Iuit I'l'leasl' of its COlllellts.

(lJ Jd t!ln.~! ullits (jato), <'less ..t ('Tp/osi/'"s: )'U\ I.-,·t "".!') 1'-", du.,s ..t ,'.flifusires: igllit.'rs, jl'l II/"'Is( IjG/UJ. duss .·1

e.rplosi:·,·s: d I/t! 1';11 it'·fS. )'uCkd .'lIt,t" 1',

class A .'J'l'/usln·s:

<I) Jl'I ll1rll:'t unit ..: (jalO). class :\ ,·x·

plosir,·s. arc IIH't:Ll c~'liJlclt-rs ('Ollt ai,I'

ing a mixture of chelllicals capable of

burning rapidly alld producing cOl\siderablt' pn·S:"lr,·. Ullckr .I·,'rt.ain cOJlditions till' ('!I"Jlli':al fut'! witt1 which t.hL'

unit is lu:ltkd Ill:IY ,·xj>lud,·. .Jd thrust

units are dt'si~lled to be il~nitt'd by ~ln

electric igniter. TIl,:~' an' used 1<) a..<;sisl

aeroplaill's to takt· "if.

I:!) !{d('Kl·t. n.ot or cla-..- A ,·,:;),t.':,i\·,:s,

is :l dt·\·jcl' rontn nuu: .. ;ll'n;".Ili:lg

dta!'~" and t'(,nsist llg of <):1" or mor«

t'tJJ1liIHltJ~L'; type con.Lu.a r-»: LI~iv.·;)

c-!u;it'd at. ull,' t.'!lel vctosur.: :.:·l:: 1>,. .cn

ig n itcr "'\'lth a t h rust pl~~tl'J ,~I~~! \s,·~th a

nO:::.'.!>:·{S):ll t hr- ot lu-r ,,!,'!. ,':.":,' r(',·~:('l

lila Lor carr ies It.:; own "·;!id u:-.:di;'.l·rrUt'l corubmat ion.) 'I't n- jll'lliwllint-:

ct mrge consists of a I11IXll.rt, .jj c1:':ll1icals :lnd.-'or cl\l'l11ical (;,HIl;)()Un,:s

which \l, hen ig n.Led is ('ap:_~i,' ur burn,

illli !':lpic~ly and produciru; ro ns.derable

pr"ssurt' :1I1d which \\ ill xuxt a i n a dvt.ona t.iun. Rocket motors. Cj:1SS A c x plosives, ,;l~ould be nonpropvuxive in shipnu-ut (.St'C par:tgraph.s (l)C!) (il and tiil

uf this sect.ion). Rocket mot.ors, c lass A

ex p losivcs. art' dt'.silo:llCd t.o )w ignitxd

by an l'lcclrically al': !Jat.ed device

which m:ty be an il£nit(·r. or by other

uu-an». Tt u-y art' used to Pi'll!,"! and/or

pl'u\'idt' t h r uxt Ior gUidl'd ::lissi!es.

rockt-tx. or xpacr-craft .

t i) A rod,t'l. motor to lJ(' l'l;nsidl.·rl'o

"uonuropulsiv.-" must i)(' '::O;J:,!Jle of

u nrr-st.ru inc-d burniru, and ',\ :11 not.

ruove apprt'ciaLJly in u uv direction

whcn ignitt:d b y any mr-nns. Blast def1l:et.ors, thrust ncutruli.x-r.. or other

shu i lu r t!t'\'ict's must !J(' p rrivi-n adc-

'luaU' by test. prior to au t lio riznt.iuu

for uxe.

eii I HOcKt·t. moto rx, cla"s :\ ,":plosi\'C's

Illa~' tJ:' sJIipP"d in a pr";'"l:;i,',· s:.ate

unl:: u nchr ('o:ldilions :lj;jll't ":i'd by till'

I), p:uunellt of Dr-Ir-ns«.

\:1) I~lliu'rs, jet t.hrust '~;t!'J;, <:I:,::os A

,·xplosin's. :tnt! igniters. !·u,·~:"t. :notor,

':L:s:.; A ,'xjJlo.-;:,·cs, an' dt'\·j(·,·" consistiii!'. oj all t'!t'('tricall~: 0;>. :'ai, J or rel:lllt,·I.\' l'Olltr"lkd ihnill'.'!: t'!t'nll'nt

a:lll :1 (·har!',· of faOil-uur:I:!!:' "\I:nposi-

: JUII 1I:1.','ling till! d"finil iU:l pn'sccribt'd

for Typ,· I ('Iass A ,·xplo:.;j':"., . ';(".' :)ar;,-

~1-a;)l1 tal uf t!lis St!/.'tiO!!J. as.,emUled i!!

:t :,nil fur us(' in ignil i::~ ~1I1' prol)l:I1:1;<'; ('l1arl-:(' of jeL t.l::';l.'.~ lllll!.:, or

l"lI'kd 1ll1l!.lIrs.

, u \ {',"IlTcJ('(/ ol! u'f'.'l /1.' ,n,·..... ·..·qLli:zfJ

.;1::.... {·II:lr;.:('d oii ·.···11 .I": ;)"I'I'Jr:Ltin!-:

,:::11:; ;([l.' stt'e) Lubt's or I::,.'!.,llit' st rips

Iidu 'xlIii'll art' 1,,,;,'!'I ..·d s!l:tpcc!

e:largt's ('olll1l't'll'd i!! :'l:·:'·S 11:: prima-

:~l)rd. Shaped rhar~('s 1'::1:." b(' of :l

t \'p,. dl.·s(·riht:d in para"T:Q,11 (11)( 1) of

Lids Sl't'tiOll, exc,'pl t II:" l'~I('l1 shaped

clrar,:!' illstallt-d ill tl\1' st,:l'l tllUI' or

l'lt'Lalli,' stl'lp sllall <.'Ullt:Lil~ not O\'c:r 4

C-9
, . i /-'\.'-'" .'" ,'.,.

ounces of high c xulostvc. Chan:,"1 nil

well jet pr-r Iorat i ng guns m uxt 11'" !ll"

trunsport.cd Wil11 bl ast irut r:q>:,. l'!r'r'! ric

blast.ina cars, or ot.hcr Iiriru: c11..\'jrl's

affixr-d to or installed in {11.~ ":1::\".

(r) Type .'J. Propellant (':''':'''';\'''''.

cla.<;,'; /t, are solid chemicals or ..;"lid

chcrnica l mixtures which an' C1o."·'I;:I<"~

to function bv r;jpi(~ CO 11111ll:, I i'II1 "f

successive layers, lcc:wral!.v ,,\jill Ii: Il!'

or nn smoke. The combust ion is (·nl.·

t r o llrd b,: composit.io n. sii''''. and fIll'::;

of r:rain. Propellant cx ploxivex. CllL';:, A.

include some tri)l'S of .·;nlnkf'I,',';.'

powder and some types of solid prilpl'l·

lant explosives for jf't t h r uxt. unil".

rockets. or ot.hr-r d('\·i(~f's. AI1~' pr"i"'!'

lant exploxivc is class A which elf'! f).

nates in anyone out of Iiv ... t ria l..

wlu-n tested in t he pnckrurr-s in \\'11kll

it is offnrcd for t ransport.at ion. ln condueling the test., one propr-Jlan; container shall be surrounded uy hu-rt

loaded cont aincrs of the same \','('j..:l1l..

incl uding one inert. corn ninr-r pl:wl'd

on top of the propellaut. cont.aincr.

ThE' propellant. shall be irmit.cd bv

means of a commercial e lect.ric squib

placed within 0\ inches of the bot torn

of the container, The pr.-sr-nr-r- of a

crater and abse-nce of fl amI.' "llal1 \)f'

considr-rcd a." evidences of dc t.ouat.ion.

Non: 1: The dr-t.onnt.lon u-st is lJ('rforJ~1C'd

by pladng Lll" sam plr: ill nu opun-r-nd fib('r

tube which Is SI'1. on t he ('no of i' Ic-ad hl"rk

npprox imatr-l y l'~ tnchr-s in diamr-t cr and 4

inches high w hich. In turn, is pla.... d ,," a

solid base. A stf'l'1 pl:1.',(' may hI' p:ar,.,j ',1"

tween tlll' f iber t nbr- and (he It'f,r1 hi"d:.

Non: 2: 1\ No. R I.'st bla.stillg' rap I' ('11'

cont a inin,: \"\'0 grams of a nux: lire' of Bll P('f·

cent rncrvu ry Iu lmtu a tc anti 20 prr(',':11 ;)1)'

la..ssiu m ch lorate, or a Utp of 0qlJ:\:dt'r:l

strvng t.h.

NOTE 3: "Uru-oru inr-d" as \lSf't~ in I 11:.;:; ~;n"

t ion litH'S not t'\,'!uc1c t lu- u:... p l): a j':,;,"r ,~r

soft fib.:r lube ..... rapping 10 laci)it"I,';' '·t,;.

N0TF. 4: TI1I' Burr:);! of Ex p losivrs )!;)I1'''o,

ApP:lraltJ~4 i:; :l tl'~tin,:: rlevin' (k~il::',I',l ..n

1.11:1.1. :l ~Ilidt'd H·pound wcin ht rl1a)' 11,-

IIro\lp<'d Irom p1'l'cktf',n,inl'o lwiv.hl., ~() '1.,

t o ill:p::ct spf'('ific Qtlnnliti('~ of 11·1':i(~ or

solid mat.r-rials unrlr-r fl Xl';! condit io ns. I)",

taill'd print < /11;.:: h,' Ubt'til1t'cj frlll" the

nllrl':\11 of Explosi';"". 1920 L :';'r""I. x.w..

\Va.slti!\f;tol1. D.C. ::,)1):16

Non: ~:~cc § 17:1,100 (gK) ior crit r rin "lal

ol't.<:rmine wllf'thrr a particular 1)'p.. "r 01,'1,

Ollalor ('an h(~ C'1~;s('d :1..': a CI:v,,, (' f. ·'i'~,,~·d'\('.

NdT>: 6:SI'l' j 173.100 Il1h I for rril'·r::t. l~.,.t

(Irlt'rl11illl' wl,,'t.hcr a pani,o'da; 1:;,'" .,! ,!rt·

C-IO

on at iru; pri:1~~·~· ';\:i h· I~la ~:"t'd :\_, :1 (·!':L·,' ("

,· ...:plnsl\"('.

: ~fI FH IP.'1~~, 1"';"'·. :!!l, : !j,; t. :IS ;i:~11'I~d' .t !1\"

(lr<lf'r 7~. :~J FH. t;4::::t, .\;ir. ,::~. ]~I"';. {Ir·j"r

";1. :n FH 90r~~, .]lI::,' ~. j~),~j; l?t>d' ~;l:n:1~!'d

;It '(:~ FH, 5~;()fl. :\\\0' ;', 1~11;':;

:~(,n:, I,'fl!" :l:lIl·11d::H.. ··

i,:,: or cFH St·~':!.':'· :,,'

11:- F:l:,Hri~: :~:d
ams Administration § 173.8'3 § 173.88 Title 49-Transportation

CLASS B EXPLOSIVES: D~;f'[N[TlONS

!lI73.ill! Delinition of class II expluxive«.

(a) Explosives, class B. are defincd a~

those explosives which in ge ncrru

Iunctlon by rapid combustion rat her

than detonation and include some e xplosive devices such as special tircworks. flash powders. some lJyr()tt'e~l'

nlc signal devices and liquid or solid

propellant explosives which include

some smokeless powders. T'hesc exutoslves are further specifically described

in paragraphs (b) to (g) of this section.

(b) Ammunition for cannon wltl:

empty projectiles, inert-loaded prok-ctiles, solid projectiles or without projectiles. or shell. and catapult charues

exceeding 2 inches in diameter. ~s

fixed ammunition assembled m a unit

consisting of the cartridge case con- talning the propelling charge and

primer with empty. illert.!oacjed., or

solid projectiles. or without projcctiles. which is fired from a C3ll,lllill.

mortar. gun. howitzer or rer-o il h-ss

rifle.

,~'." (cl Rocket ammunitioll !s fixed am·

~\i~~i\nunltlon which is fired frolll a tU:'t'.

····'s:~;uncher. rails. trough. or other deVICt'

as distinguished from cannon ammUIlI·

tlon which is fired from a cannOll, gUll,

or mortar. It consists of an igniter, a

rocket motor. and empty prokctile.

inert-loaded projectile. or SUlld prUjl"'·

tile, I'

(dJ Special fireworks are manu aetured arUcks (!<'siglll~d priluanly Illr

the purpos(' of producill~ visiblc' or au·

dible pyroLechnic effecL..; by cO!llbus·

Lion or l'xplo.siol1. (See § l7J.lOO(rl for

common fireworks.) Examplf's arl' loy

tOfJwchws. railway torpl'c1C)l'S, , SClIlll'

firecrackers and saluLl·s. ex 111blll0l1

di,5play pieet·s. aeroplane Clan'.,. Illuml·

natin!: prokct.ill~s, incendiary pn~jC:c,

tiles inc('ndiary bombs or II\C'l'lldlary

grell'aucs alld .smoke proj"cLilt-s or

smoke bombs fuzed or tlllfllz,'d :1I1:1

containing expelling chargl's but \\"iL~:­

out bursting charges. f1a.'>h pow<lt'r:; III

inner units not exceedillg 2 llune,·s

each. flash sheets in interior ;JacKagCs,

flash powder or spreader cartJ'I.dg,·s

containlnJ.; noL over 72 gr:lins of lIasll

. powder each lsee § 173.60 .for ShIP'

ments made as low CXpIOSIH:S) and

fla.~h cartrictt~('s consisting of a I,apt'r

cartridge shell. small·arm.'; pril11l'r. and

flash C'(j1l1PI,;dtitln, not. l'xe""dilll: 1:\(1

grains ;;,11 asxom blcd ill O!\I' pil'c('. Fin',

works must be in a finishnj st a t ». ,,:.:.

elusive of !ll('rl' ornnm.-nt atlon. ;,,.: .;~,;!.

pl icd t.o thc' rdai! trade and mus: I),' ;;"

const.rurt ed and packed tint. Ioo.« I'y.

r ot cclmic composition will 1I0t. b" 1'1"':'·

"IIL in p;1.('kaf~(.'s in l ransport at in11.

lr) .JC't. t hrust u n it x r ja.t.o i. rla.';s II /'\.

nlosivcs: ro..-kot motors. r laxs n '·:,I';tl·

sivcs: igniters, kl ,Ilrusl tiat o ). ";:~ 'c' il

e-xplosives: and igni~crs, rocket I1w,nrs,

d,1."S B cxptostvcs:

(1) Jet thrll:;t units (jato). cl:1s.'; l\ rxplosivcs. are met at cylf ndr-rs ('onl a iniru; a m ix turc of chrm ica.ls ('ap:1"'" 'If

burntna rapidly arid nrodur-uu; {'OIL' ,d·

erabt« pressure. JeL thrust units ,Ul'

(\C'sig-Ill'r! to !H' il~nitC'd by an l'1l'l't rir il~­

niu-r. Thl'Y nrr- usr-d to nxxist .u-rnpln nr-« to t:lkl' off. .

(21 l{cwkl'll!lotor, rlnss B l':,<pIO":I\'-·;',

is a d"vict' cont.a iniru; a propt'llil1l:

chargC' and ('on:.;i;;1 iru; of 0111' or mill'"

continuous type r-ornhust ion unius i.

closr-d at. one end (closure mas Ill' :1.11

ic nlt.cr wit h a thrust. platc~) and wit h a

nozz.lc: s ) at Uw ot.her cn(1. TI1C' proppJ·

lilH: charhl' consists of a nlixtlJlT of

chemicals and/or ehemical cornpnuncb

which wlH~n ignitt'd is cap:1hk of bUfn·

ill!: rapidly :1IHI prodllcing ctlnsicl''I":1iJl,'

pressure and which will not. sustain a

dl'tollaLion. lThC' rockl't. mol or C:1 rri,':;

its own solid nxicli7,C'r-fup! cOIllbina·

Lion. i H.od:l't mot.ors, cl:1s:; B ('xplo-

::ivcs. should be ;lOnpropulsin' in (;h:p·

ment. (sec paragra.phs (e)(2i Ii) and 'I;'

of this sl'ctioni HockC't motors. r!;l:-S n

explosivl;S, are desil:ncd to lw h:n:t ('d

hy an plC'nriC'ally actllH!l·t! d/'\'icl'

whirh may bC' all il'niter. or by oi l)('~

mea.ns. Th'cy arC' used to propC'1 and.' til"

pro\'ic1C' 111~ust for guicl,·(\ I11Ls:,iks,

rockets, or ;,paC('t'r:1,(t.

(i) A rockr·t mol or 10 ht' cnn(':idl':'·.J

"nonprnpulsi\'l''' must bl' c:apahl,' 0f

unrestraincd burning and wil! ::n'

mol'C' apprl'c'iably in an:; dil"l'C'l in:l

..... lll'n igni It'd by any means. Hla:;! rj"oflectors. thrust ncutrali7.t~rs or 0111t'r

~imilar c1C'\'ircs must hI' pro'. l'l1 h:; I"s\

prior Lo :1.utl1orizat ion for liSt'.

ilil Rockf't. motors, CI:1sS B l'xpln.

sin:s, may 1)(' shippf'd in a propulsl'"''

slat.e onlv under conditions appro·;l.'d

hy till' o','p:lfln1l'Ilt of Del"l1s(' or till'

National Acronautic~ a ncl SpacC' i\ O!.

ministrat io'1.

C-ll

,:11 Jgllilt'rs, j"l thrust (jato), class B

rx plosh'(':<, and ignill'rs. rocket motor,

t'i:l.SS B ('xplosj'''''s, nrr- devices consist-

::I? of a.n "ll'('1ri":1,11\' opf'ra.tl~d or rr-..

ruot rlv control lcd il:ni: ion element

:1,,(\ a' Iast hur-n inc cOll1lJl·sif.ion which

'In,ci ions b:: r:l;lic1 bllt'uillg" rather

. 'I:,:: dr't.nr1:1t.itll1, ~1..s.'<t'tnlJkd in a unit

'",. ,:s(' :11 ig:iitilll: t h- propC'lIing

<Iart:!' of .iel thrust. units. rocket.

Tllut ors, or ,-ocker ('nl-dnes.

'I'I l'r"il"lInll! r.rp/nsil'f'S. ctass lt,

Pronr-Har.t ,~xplosi·;(·s. r lass B, are so~id

or liquid chr-mtcats or chemical l~lIX'

r urr-s which :llnet ion by combust.ion.

Tile comh:l.«! ion L.; r-ont.rnllud by cornposit inn, siz«. Iorrn of gr:1ill, or othcr

chl'll1ical or rn or-hn.ntcn l means. Any

propellan( is e lass B wh ich fails to dotnl1:,,(' in fh'r t.rin ls when t.ost.ed (Sl'r

1'ott' :n in tlu- par:k:1 gl' in which it is

oCff'r('c! for sl upmr-nt. Propellant ex111nsi\'('S, cl:',,:,~ B. :Ilt-lud" smokr-less

I"lwrkr for small arms (:;l't' Not." 4.).

:;mokl'lt'ss powdr-r .jor r-a.nnon, llqnld

mo nupropc llunt fl1l'1 (.'>t'r. Note 3),

smokctess powder. or so lid propellant

cx ploxivr-s for rrick et s. ,it't t hrust, units,

or other devices. Ulack powder is not.

included in this cla..,,::;ific::1t.lon and is

e!dinC'd spl'cifical1~' in § 17:\.:1:l.

(l!) Explosives p'Jwer dl'viccs, CIR..'>s

B. arl' dC'\'icl's c!C'signC'd 1,0 operatC'

(' ject ing apparat.us or other mechar;isms by Ilit'ans of 'a propdlant explosi\·C'. Cla.."s B. ane! r.Lffl'r from rxp!osive

power dc\'ices, CIa-,s C. in that they

co!'tain larl-:"C'r or !1101't' powerful pro·

pdlant.s. The de\"icl's 11111:,1 not ruptllre

Oil fUllctioninl' and must be of a type

l'xamin('c\ b~' the BllfC'au of Explosives

:1.lld approved hy t.he Associate Direct or for OE. ('xcC'pt a." ot.herwise pro-

\'ided in § 1'73,~1(a}(16) and § 1'73.86(a),

Non: I: Firo'-t''(: in;:l!isht'r l"h~,rr.rs cont.ain·

il\>: nOl 10 t'x"rcd 50 gr~in~ of prupellant ex·

plosiv!':: 1)('1" l!lli! :lrl' ('xcrnpl from the regu·

l:l:ions in Pa:',,, l'iO-IR!\ of 1his rhapter.

Nnn: 2: In .."ndllt-tin~ I Ill' !('~l. one proppl·

i",nl eOIl:"ilwr shall bl' Sllrrounrkd by inert

;nadpd conlailll'I"S of the sa.me wf'lght. in·

rillcling on,' 111l'rt ,:t>lllainn placl'd on top of

lht' propt'II""1 conl"int'r. The propellant

:;I):lll b,' il:l:llrd b:: n1l'nns of a commercial

I'kctric squib pl:1 r ",1 \l'ithin 4 inches of the

bl)1 tom of l h,' conI :lirwr. Thp. presence of a

cr:lt('r and abspnr(' of nanlf" shall he consid·

I'r"d as p\'id"nrps of tlf-t Oll:lf ion.

NOT!: 3: A liquid mnno;>ropcllant fuel is

odinI'd as any propt'llant in which the fllel
:.ll.d t!ll' ux:,-:iz·:r art' jl:l:, -, jt .~:::~. IIr t'l1l:. ::1l(":~!'

Iv (,o::.b;:I~·d If. nne rorr».

. NUTt.: 4: S:n'Jkl'lf·.s." pu'., ~l"r fdr ~.Jllall a!"l:i:i

in (;l~:ln' I~il'~ nut {·:-:l.···d.:!;.: lll~) ;H)'::l.:b ::t·:

;;~/;~J\I:~",~~~ I~~~.' ;~;l\:. ::~. ~:l~··:~i·.·~.. i~~i::.':~\';l:t:~:~t'~;~. tilt' Arrn y , Navy, or .·\ir l··I.I"L·l' 01 l i u- l:~.i·.l'd

St.~(I·.'" CiU',I'ITiiJH·IH. :.~I:L:: l.it· rl.. ........ l:: .t... a

fla:r..:nablt· so l id lor pur~_hlsi'S 0: tr;111~;}On:t·

t ion '.1, ~ll'n pr..ckaged i:l :H·(·ort.!.t1!{·,.· ....Il. !;

17:i, J ~7;1.

ill) :c: t.art 1'1' canrid~:t:.< jet l·lItdll<:.

cl:L':.' II l'XplO:ih "s cOll.,:ist of p!a:il!c

and: or rubuer cast's. ,':tell cout.a ininu a

Pl'('s:<<:d vyl indrical block of propellant

oxptosiv..· a nd havin., in th,' top uf t lucas", a smal! compnrt nunt tllat ill'

close-s an ..lectrica! .';l;l:ib. small

amounts of black powde-r. and s.nok«

less powder. whic h CUI1<:lutcs all i>;,

nite-r. TIll' startcr cartr:·h:c is u::,·,j t o

acuvau- a mccluuur-a: ,,1;lr~,'r 1'1';- .Il'l

erig iru-s.

(j) Rock ct c'ng"ille t l lq u id ). clnsx Is r-xplosin';; I:; a COlllpll'll'. St'!f,collcainl'd

rocke-t propu 1:.,: on un i[ wl1ich con tu iIlS

an nxidiZt'r and :1 fuel. each scuara t cd

by a n :t111I11i!1l1l1l or ~;I :lillit'S:; ;;t"", w.i ll

of not I":i:'; t hnn O.~!)(J illr:ll t h ick ru-ss.

D',lll,j(, walls aI'" 1H'r111 iItl'd. 1'[('ssur,

iZ:lli(//1 of tile propr-Hant t a nk s is by

USt; of a f:a.'i gt'!wr:\[or. Tilt' I~:nil ion

:,Ullr('(' I:llt:: IJ(' ill all uu.uuu-d PUSitiUll

fur ...,lriJiJl~'·lll. Rud.t:i '!l,!inl's (liquid)

:,rL' ll:il'll to prUIJl'! or providc thrust

fur ruf·kt·~s. JIl:"i."il,':) (:1" ·..;pacccraft.

j ~~! }-'H j .;c;K:_~. 1)l'{·. ~:J. ! ~l/i·l. as- :i.1I11'!It.kd by

unh'(' 'i.:, :$: r:'H jj.;~.\, :\;)1'. :2K. l~jjti. Hf..dt·s-

:,'l .. d. d al :L~ l"I~ ~,'j!:I: . ..\jJJ". :'. l~"j·i. <LIlli

:,::.·.·lllh·d t,~ :\nHII. l''';) ~lJL 4~ 1-'1 { 11:!:~!J.

'·"·!l. ::B. 1,)'0'7: :\llIJI I~:I UK. 4::; I·'n 3::ti!H.

[\l;t:; ! ~I 1~,lHlI !

C-12

..--..
_.-.....,

APPENDIX 0

EP TOXICITY TEST

Procedure

1. A representative sample of the waste to be tested (minimum size 100

grams) should be obtained using methods capable of. yielding a r.epresentative sample.

2. The sample should be separated into its component liquid and solid

phases using the method described in "Separation Procedure" below. If

the dry weight of the solid residue* obtained using this method totals

less than 0.5 percent of the original wet weight of the waste, the

residue can be discarded and the operator should treat the liquid phase

as the extract and proceed immediately to Step 8.

The solid material obtained from the Separation Procedure should be

evaluated for its particle size. If the solid material has a surface

area per gram of material equal to, or greater than, 3.1 cm2 or

passes through a 9.5 mm (0.375 inch) standard sieve, the operator

should proceed to Step 4. If the surface is smaller or the particle

size larger than specified above, the solid material would be prepared

for extraction by crushing, cutting or grinding the material 'so that it

passes through a 9.5 mm (0.375 inch) sieve or, if the material is in a

single piece, by subjecting the material to the "Structural Integrity

Prot:edure" described below.

The solid material obtained in Step 3 should be weighed immediately and

placed in an extractor with 16 times its weight of acetic acid-sodium

acetate buffer.~/Do not allow the material to dry prior to weighing.

For purposes of this test, an acceptable extractor is one which will

impart suffucient agitation to the mixture to not only prevent stratification of the sample and extraction fluid but also insure that all

sample surfaces are continuously brought into contact with well mixed

extraction fluid.

s. After the solid material and the acetic acid-sodium acetate buffer are

placed in the extractor, the operator should begin agitation and

measure the pH of the solution in the extractor. The mixture should be

agitated for 24 hours and maintained at 200 - 400 C (680 - 1040 F) during

this time.

6. At the end of the 24 hour extraction period, deionized water should be

added to result in a solution 20 times the weight of the solid material

obtained in Step 3.

~/ Use 0.1 M sodium acetate/O.l M acetic acid.

*The percent solids is determined by drying the filter pad at 800C until it

reaches constant weight and then calculating the percent solids using the

following equation:

(weight of pad + solid) - (tare weight of pad) X 100

initial wet weight.of sample

D-l

% solids
.r">.....

7.

.~.

The material in the extractor should be separated into its component

liquid and so lid phases as descri bed under "Separ at ion Procedur e."

8. The liquids resulting from Steps 2 and 7 should be combined. This combined liquid (or the waste itself if it has less than 0.5 percent

solids, as noted in step 2) is the extract and should be analyzed for

the presence of any of the contaminants specified in WAC 173-303-090

(8) using the procedure for analyzing the extract given below.

Separation Procedure

Apparatus

A filter holder, designed for filtration media having a nominal pore size of

0.45 micrometer and capable of applying a 5.3 kg/cm2 (75 psig) hydrostatic

pressure to the solution being filtered shall be used. For mixtures containing nonabsorptive solids, where separation can be effected without imposing a

5.3 kg/cm2 pressure differential, vacuum filters employing a 0.45 micrometer

filter media can be used.

Procedure*

1. Following manufacturer's directions, the filter unit should be assembled

with a filter bed consisting of a 0.45 micrometer filter membrane. For

difficult or slow to filter mixtures a prefilter bed consisting of the

following prefilters in increasing pore size (0.65 micrometer membrane,

fine glass fiber prefilter, and coarse glass fiber prefilter) can be

used.

2. The waste should be poured into the filtration unit.

3. The reservoir should be slowly pressurized until liquid begins to flow

from the filtrate outlet at which point the pressure in the filter

should be immediately lowered to 10-15 psig. Filtration should be

continued until liquid flow ceases.

4. The pressure should be increased stepwise in 10 psig increments to

75 psig and filtration continued until flow ceases or the pressurizing

gas begins to exit from the filtrate outlet.

*This procedure is intended to result in separation of the "free" liquid

portion of the waste form any solid matter having a particle size >0.45 pm.

If the sample will not filter, various other separation techniques can be

used to aid in the filtration. As described above, pressure filtration is

employed to speed up the filtration process. This does not alter the

nature of the separation. If liquid does not separate during filtration,

the waste can be centrifuged. If separation occurs during centrifugation,

the liquid portion (centrifugate) is filtered through the 0.45 ~m filter

prior to becoming mixed with the liquid portion of the waste obtained from

the initial filtration. Any material that will not pass through the filter

after centrifugation is considered a solid and is extracted.

D-2
s.

...-....

The filter unit should be depressurized. the solid material removed

and weighed and then transferred to the extraction apparatus, or. in

the case of final filtration prior to analysis. discarded. If the

solid is to be extracted. do not allow the material retained on the

filter pad to dry prior to weighing.

6. The liquid phase should be stored at 40C for subsequent use in Step 8.

Structural Integrity Procedure

Apparatus

A Structural Integrity Tester having a 3.18 cm (1.25 in.) diameter hammer

weighing 0.33 kg (0.73 lbs.) and having a free fall of 15.24 cm (6 in.)

shall be used. This device is available from Associated Design and Manufacturing Company. Alexandria. VA •• 22314. as Part No. 125, or it may be

fabricated to meet the specifications shown in Figure 1.

1. The sample holder should be filled with the material to be tested. If

the sample of waste is a large monolithic block. a portion should be

cut from the block having the dimensions of a 3.3 cm (1.3 in.) diameter

x 7.1 cm (2.8 in.) long cylinder. For a fixated waste, samples may be

cast in the form of a 3.3 cm (1.3 in.) diameter x 7.1 cm (2.8 in.)

cylinder for the purposes of conducting this test. In such cases, the

waste may be allowed to cure for 30 days prior to further testing.

2. The sample should be placed into the Structural Integrity Tester, then

the hammer should be raised to its maximum height and dropped. This

should be repeated fifteen times.

3. The material should be removed from the sample holder, weighed. and.

transferred to the extraction apparatus for extraction.

Procedure for Analyzing the Extract

The test methods for analyzing the extract are as follows:

1. For arsenic. barium. cadmium. chromium. lead, mercury, selenium or

silver: ''Methods for Analysis of Water and Wastes." Environmental

Monitoring and Support Laboratory. Office of Research and Development. U.S. Environmental Protection Agency. Cincinnati. Ohio 45268

(EPA-600/4-79-020, March 1979).

For Endrin; Lindane; Methoxychlor; Toxaphene; 2,4-D; 2.4,5-TP

(Silvex): in "Methods for Benzidine. Chlorinated Organic Compounds.

Pentachlorophenol and Pesticides in Water and Wastewater." September

1978. U.S. Environmental Protection Agency. Environmental Monitoring

and Support Laboratory. Cincinnati. Ohio 45268, as standardized in

"Test Methods for the Evaluation of Solid Waste, Physical/Chemical

Methods." For all analyses, the method of standard addition shall

be used for the quantification of species concentration. This

method is described in "Test Methods for the Evlauation of Solid

Waste." (It is also de s cr Lbe d in "Methods for Analysis of Water

and Wastes. ")

D-3
APPENDIX D

FIGURE

EXTRACTION PROCEDURE FLOWCHART

Representative

Wet Waste sample

contains < 0.5%,/

non-fllterahle ~X--I

solids

Waste Sample

> 100 grams

Dry Waste 5anple

Wet waste Sarrple

~oontains > 0.5% f---~7 n::>n-filterable

solids

1

Structural

Liquid Solid

~lid~--

Separation ~lfd

Discard

Particle size

> 9.5 nm

~~. < 9.5 mn nonol1.thic

Separation

Liquid Solid

sample Size

Integrity

Reduction

Procedure

Store at

> Extraction of Solid waste "'

4° C aril/or

at • = 2

Solid f--

Discard

1

Liquid Solid Separation

..t

Liquid

{

EP Extrclct

!

l\nal}'9is Me~

n-4
.....~~;}-_ (3.1Scm)

(1.2S")

(

7.1-11

1

SAMPLE

ELASTOMERIC •

SAMPLE HOLDER

COMBINED

WEIGHT

.33Kg

(.731b)

1S.2Scm

(6")

7.1cm

(2.8")

~~l

*ELASTOMERIC SAMPLE HOLDER FABRICATED OF

MATEt:lIAL FIRM ENOUGH TO SUPPORT THE SAMPLE

Figure "

L

COMPACTION TESTER

D-5
7.5-4

:-....

.: .. ".: ...... ,

1

9.0

5.00::1

-r~ 2S

.\ ,\ '.\\\\\\.\'l . !f'\\"\\\\\\\'. 1

4.0

NON CLOGGING SUPPORT BUSHING

1 Inch BLAOE AT 30' TO HORIZONTAL .

Figure 3 , EXTRACTOR

:' .~.-:-\

. '. "-.,/

<.

D-6
,-

\.

..

•

2-1iter plastic or glass bottles

lllS horsepower electric motor

-- . " I" (

screws for holding bottles

Figure 4

BOI'ARY EXTRACTOR

,.....

I

l=l

ec

, ,

c: ,...... ,A',

4fk;--:" rA"jJ

.~··!:i4 ..1

_._---_.. --_.~-------'.

,

""')'

.'. ~~
.-", !

) . "

Foam Inner L1neet ,

I

Q

Box Assembly

Plywood Construction

Foam Bonded to Cover

I

;/

Figure 5 .

EPRI/ACUREX EXTRACTOR

,........\-."....

(-.:~~i~ ..>:..J O

(

---;;;;;;. I

I @ r

3 Position Toggle Sw1tc~

..- .' ( "

\ .

l-gallon plastic

or glass b~ttle

( ,

(

•
APPENDIX E

.:~

CRUDE SAMPLE EXTRACT ION FOR HALOGENATED

AND POLYCYCLIC AROMATIC HYDROCARBON ANALYSIS

The crude sample may be in several physical forms and mixtures of these

forms as follows:

1. Dry grandular solid.

2. Solid with liquid organic phase.

3. Solid with water phase.

4. Large chunks of a tar-like solid material.

5. Liquid organic phase only.

6. Water phase only.

7. Solid granular phase that is damp with water.

8. Combinations of the above.

Each of these physical forms may require different extraction procedures.

Therefore, in many instances the extraction procedure or combination of

extraction procedures that will be used are the chemist's best judgment

when he receives the sample.

The extractions of single phase sample systems are covered in the following written discussion. The multiple phase systems would be separated by

decantation, filtration or centrifuging and each phase then treated as

a single phase system. For all procedures about 10 grams (accurately

weighed) of crude sample is used.

Extraction of a dry granular solid - the sample is extracted (18 - 24 hrs)

with petroleum (pet.) ether, using a Soxhlet extraction apparatus or by

stirring (over 18-24 hr. period) the sample with three successive volumes

(approx. 20 ml) of pet. ether and decanting. The pet. ether phase from

these extraction procedures is Fraction #1 in Figure 1•

. Extraction of a liquid - the sample is extracted by shaking in a separatory

funnel with three successive equivalent sample volumes of pet. ether. The

pet. ether phases are combined and again labeled Fraction #1.

Large chunks of a tar-like solid material - the simple extraction of an

organic sample with petroleum ether does not always give a complete extraction of the petroleum ether soluble components. This is especialiy true

if the sample is of a tar like consistency. The petroleum ether easily

removes the petroleum ether soluble components from the surface of the

chunk. Rowever, when the surface of the chunk becomes covered with a

remaining layer of petroleum ether insoluble material, the extraction of

the soluble material within the body of the chunk slows down and nay even

~' come to a complete halt. The extraction time and/or chunk size are the

controlling factors in obtaining a complete extract from the sample.

s-t
, .'-./..

J

To prevent extraction time and chunk size from becoming controlling factors,

all of the soluble organic material should be dissolved in a solvent with

more complete solubilizing ch ar act erLstt cs for the organic material.

(Example: CH2C12 - df ch Lorome t hane, ) The solution is then poured over

an inert particulate such as sand. The mixture is stirred to get a uniform

thin coating on the sand as the solvent evaporates. The organic coated

sand is then extracted with petroleum ether by the Soxh1et extraction method

or by stirring the sand with petroleum ether in a closed flask.

Solid granular phase that is damp with water (see Appendix E, Figure 1) -

to insure a good solvent wetting action of the material, it is extracted by

shaking three times with 20 ml portions of solution containing 60 percent

isopropyl alcohol and 40 percent pet. ether. A fourth extraction is made

with 20 ml. of pet. ether. All extractions are combined. Inorganic halides

are somewhat soluble in the alcohol/pet. ether solvent. Therefore, the

solvent extract is further treated to remove any inorganic halides before

testing the solution for organic halides by the Parr bomb organic halide

analysis procedure. To accomplish this, the solvent extract is poured into

a separatory funnel and two solvent extract volumes of water are added to

break the alcohol/pet. ether solvent phase. The alcohol-water and pet.

ether phase are separated. Another volume of water is added to the alcoholwater phase. The alcohol-water phase is extracted twice with 20 mI. volumes

of pet. ether. The pet. ether phase is washed twice with 20 mI. volumels of

water. All water phases are discarded and the pet. ether phases are combined and saved. Now the pet. ether fraction from the alcohol/pet. ether

breaking procedure is washed twice with 20 mI. of water. The water extracts

are discarded and pet. ether phases are combined with the pet. ether extracts

saved from the earlier pet. ether washes of the water-alcohol phase. The

combined pet. ether solution is labeled Fraction #1 (see Appendix E, Figure 1).

E-2
~.

APPENDIX E

FIGURE 1

HAZARDOUS WASTE EXTRACTION PROCEDURE FOR ANALYSIS OF HALOGENATED HYDROCARBONS

AND POLYCYCLIC AROMATIC HYDROCARBONS

10 gm CRUDE SAMPLE

If dry .mple

_treet 3 times wlttl

~. ether (20 mi••ech)

FRACTION NO.1

If tar like aolid material:

dlaolva In wonger org.nic

eolv.nt IUch .s CH 2 CI 2 and

pour over inert particull!lte

IUch .s aand

If w.t umple

extract 3 ti".,.. with mixture of

60% iaopropvl alcohol/40% pet. ather (20 mls eech)

4th ."traction witt> pat, .ther (20 mil)

ISOPROPYL/PET. ETHER FRACTION

NOTE: Should have appro" imatelv 80 ml volume

evepor.ta and waigh

If r..ldue· > 1%

continue

Add 2 Yolum.. of water

NOTE: "Volume" r.fe.. to the totel volume

in previous step

Add .dditional volume of water

Halogenated

hydrocarbon

",aly.l.

Polycyclic

aromatic

hydrocarbon

.nalysis

ISOPROPYL/WATER FRACTION

E"tract 2 timas

with pet, ether

(20 mls each)

PET. ETHER FRACTION

E"tract 2 timet

with water

(20 mls each)

DISCARD

ISOPROPYL/WATER

FRACTION

DISCARD

WATER

FRACTION

PET ETHER

FRACTION

E"tr.ct 2 times

with water

(20 mlsaach)

COMBINE TO MAKE

FRACTION NO.1

Evapor.t••nd w.lgh

If r..ldu. - > 1%

continue

DISCARD

WATER

FRACTION

./ > .01% fOt" H. H.

r· '';

H.logen.ted

hydroc.rbon

.....ly.ls

Polycyclic

...omatic

hydrocarbon

analy.is
--',\

APPENDIX F

ATTACHMENT 1

ANSI/ASTM D808-63 (REAPPROVED 1976)

American Society for Testing and Materials Standards are protected by

copyright. Copies of ASTM standards can be obtained by writing to the

following address:

ASTM

1916 Race Street

Philadelphia, PA 19103

Steps 6.5, 6.6, and 7 in the above referenced method are replaced by

the chloride determination described in Appendix F, Attachment lao

F-l
,---..

.' ":

-:.......

:~~

APPENDIX F

FIGURE 1

HAZARDOUS WASTE HALOGENATED HYDROCARBON ANALYSIS

FRACTION NO.1

(Se~ Appendi~ E. Figure 1)

PARR BOMB ANALYSIS

Appendi~ F. Attachment'

F-2

GAS CHROMATOGRAPH

See EPA Method 612
APPENDIX F

ATTACHMENT la

CHLORIDE

Method 325.3 (Titrimetric, Mercuric Nitrate)

STORET NO. 00940

l. Scope and Application

1.1 This method is applicable to drinking, surface. and saline waters, domestic and industrial

wastes.

1.2 The method is suitable for all concentration ranges of chloride content; however, in order

to avoid large titration-volume, a sample aliquot containing not.more than 10 to 20 mg CI

per 50 m1 is used.

1.3 Automatedtitration may be used.

2. Summary of Method

2.1 An acidified sample is titrated with mercuric nitrate in the presence of mixed

diphenylcarbazone-bromophenol blue indicator. The end point of the titration is the

formation ofthe blue-violet mercury diphenylcarbazone complex.

3. Comments

3.1 Anions and cations at concentrations normally found in surface waters do not interfere.

3.2 Sulfite interference can be eliminated by oxidizing the 50 ml ofsample solution with 0.5

to 1m1 ofH202.

. 4. Apparatus

4.1 Standard laboratory titrimetric equipment including a I ml or 5 ml microburet with 0.01

m1 graduations.

5. Reagents

5.1 Standard sodium chloride, 0.025 N: Dissolve 1.4613 ±0.OOO2 g :(dried at 6O(jC for 1

hour) in chloride-free water in a 1 liter volumetric flask and dilute to the mark.

5.. Nitric acid, HN01 solution (3 + 997)

5.3 Sodium hydroxide solution, NaOH, (10 gil)

5.4 Hydrogen peroxide (30%), H202

5.5 Hydroquinone solution (10 g/liter): Dissolve 1 g of purified hydroquinone in water in a

100ml volumetric and dilute to the mark.

5.6 Mercuric nitrate titrant (0.141 N): Dissolve 25 g Hg(NO)2·H20 in 900 m1 of distilled

water acidified with 5.0 ml cone. HNO) in a I liter volumetric flask and dilute to the

mark with distilled water. Filter if necessary. Standardize against standard sodium

chloride solution (5.1) using procedure 6. Adjust to exactly 0.141 N and check. Store in a

dark bottle. A 1.00 ml aliquot is equivalent to 5.00 mg of chloride.

5.7 Mercuric nitrate titrant (0.025 N): Dissolve 4.2830 g Hg(NOJ)2·H20 in 50 ml of distilled

water acidified with 0.5 ml cone. HNOJ (sp. gr. 1.42) in a I liter volumetric flask and

dilute to the mark with distilled water. Filter if necessary. Standardize against standard

Approved for NPDES

: :~ Issued 1971

.<:> Editorial revision 1978

~.

325.3-1

F-3
.- '"""\

.'---"

.,-...,..

sodium chloride solution (5.1) using procedure 6. Adjust to exactly 0.025 N and check.

Store in a dark bottle.

5.8 Mercuric nitrate titrant (0.0141 N): Dissolve 2.4200 g Hg(NO))2-H20 in 25 ml of

distilled water acidified with 0.25 ml of cone. HNO) (sp. gr. 1.42) in a 1 liter volumetric

flask and dilute to the mark with distilled water. Filter if necessary. Standardize against

standard sodium chloride solution (5.1) using procedure 6. Adjust to exactly 0.0141 N

and check. Store in a dark bottle. A I ml aliquot is equivalent to 500 ug ofchloride.

5.9 Mixed indicator reagent: Dissolve 0.5 g crystalline diphenylcarbazone and 0.05 g

bromophenol blue powder in 75 ml 95% ethanol in a 100 ml volumetric flask and dilute

to the mark with 95% ethanol. Store in brown bottle and discard after 6 months.

5.10 Alphazurine indicator solution: Dissolve 0.005 g of alphazurine blue-green dye in 95%

ethanol or isopropanol in a 100 ml volumetric and dilute to the mark with 95% ethanol

or isopropanol.

6. Procedure

6.1 Place 50 ml of sample in a vessel for titration. If the concentration is greater than 20

mg/I chloride, use 0.141 N mercuric nitrate titrant (5.6) in step 6.6 or dilute. If the

concentration is less than 2.5 mg/I of chloride, use 0.0141 N mercuric nitrate titrant

(5.8) in step 6.6, a I rnl or 5 ml microburet, and determine an indicator blank on 50 ml

chloride-free water using procedure 6.6. If the concentration is less than 0.1 mg/l of

chloride concentrate an appropriate volume to 50 ml.

6.2· Add 5 to 10 drops of mixed indicator reagent (5.9), shake orswirl solution.

6.3 If a blue-violet or red color appears add HNO) solution (5.2) dropwise until the color

changes to yellow.

6.4 If a yellow or orange color forms immediately on addition of the mixed indicator, add

NaOH solution (5.3) dropwise until the color changes to blue-violet; then add HNO)

solution (5.2) dropwise until the color changes to yellow.

6.5 Add 1ml excess HNO) solution (5.2).

6.6 Titrate with 0.025 N mercuric nitrate titrant (5.7) until a blue-violet color persists

throughout the solution. See 6.1 for choice of titrant normality. Alphazurine indicator

solution (5.10) may be added with the indicator to sharpen the end point. This will

change color shades. Practice runs should be made.

6.7 Additional steps to eliminate particular interferences:

6.7.1 Ifchromate is present at < 100 mg/l and iron is not present, add some alphazurine

indicator solution (5.10) and acidify to pH 3 (indicating paper). End point will then

be an olive-purple color.

6.7.2 If chromate is present at > 100 mg/l and iron is not present, add 2 ml of fresh

hydroquinone solution (5.5).

6.7.3 If ferric ion is present use volume containing no more than 2.5 mg of ferric ion or

ferric ion plus chromate ion. Add 2 rnl fresh hydroquinone solution (5.5).

6.7.4 If sulfite ion is present, add 0.5 rnl of H10 2 solution (5.4) to 50 rnl sample and mix

for 1 minute.

325.3-2

F-4

(.

(

(
',-' ........

7.

'-',

Calculation

mg chloridell - (A - B)N x 35,450

ml of sample

where:

A = rnl titrant for sample

B = ml titrant for blank

N = normality mercuric nitrate titrant

mg NaClll = mg chloridell x 1.65

8. Precision and Accuracy

8.1 Forty two analysts in eighteen laboratories analyzed synthetic water samples containing

exact increments of chloride, with the following results:

(FWPCA Method Study I, Mineral and Physical Analyses)

8.2 In a single laboratory (EMSL). using surface water samples at an average concentration

of 34 mg CVI, the standard deviation was :t 1.0.

8.3 A synthetic unknown sample containing 241 mg/l chloride, 108 mg/l Ca, 82 mg/1 Mg,

3.1 mg/I K, 19.9 mg/l Na, 1.1 mg/l nitrate N, 0.25 mg/l nitrite N, 259 mg/l sulfate

and 42.5 mg/l total alkalinity (contributed by NaHC03) in distilled water was analyzed

in 10 laboratories by the mercurimetric method, with a relative standard deviation of

3.3% and a relative error of2.9%.

Bibliography

1. Annual Book of ASTM Standards, Part 31, "Water", Standard D512-67, Method A, p 270

(1976).

315.3-3

F-5
-r-:

APPENDIX G

DEPARTMENT OF ECOLOGY

HAZARDOUS WASTE

POLYCYCLIC AROMATIC HYDROCARBON (P.A.H.) ANALYSIS

Stock Pet Ether Fr #1

Extract twice using one equivalent vol. of 2N HCl for each extraction. The

water and organic layers are separated with a separatory funnel. The water

layer contains the basic components and, for this work, it 'Ls discarded.

Pet. Ether Fraction

Extract twice with one equivalent volume of ZN NaOH for each extraction. The

water and organic layers are separated with a separatory funnel. The water

layer contains the acidic components and, for this work, it is discarded.

This-pet. ether fraction which remains after the ZN NaOH extraction contains the neutral componenents, including the P.A.H. components, the

fraction is labeled Fraction #4.

Fraction 114

Dry with anhydrous N'aZS04 (Z-5 gm) , Decant and save the clear supernatent liquid. Wash the NaZS04 residue once with a small amount of pet.

ether. The pet. ether wash is again decanted and added to the first supernatent. The pet. ether supernatent is evaporated by placing the container in

a warm water bath, while flushing the container with a gentle stream of dry

N2' The residue is weighed and, if it is found to be greater than 1

percent of the original crude sample, the residue is again dissolved in ZO cc

of pet. ether.

A silica gel column (see Attachment 1 Appendix G) is prepared for liquid

chromatographic separation of the reconstituted Fraction #4.

A measured aliquot of reconstituted Fraction #4 that does not contain more

than 0.5 gm. of the dissolved residue is carefully pipeted onto the silica

gel column. The column is eluted at approximately Z ml/min. with approximately 5 column volumes (volume in the column occupied by the column packing)

of pet. ether. The eluate contains the aliphatic group and is discarded.

Fraction 116

The column is next eluted with approximately 3 column volumes of benzene.

(Caution: benzene is toxiCi therefore, steps should be taken not to

breathe the fumes.) Combine all extracts and identify the mixture as

Fract ion 116.

The benzene is removed by the same evaporation procedure used previously

for pet. ether. The residue is weighed to determine its percentage of the

original crude. Fraction #6 may consist of a major part of P.A.H. compo-

.~ nents that are not of concern, such as Naphthalene, Anthracene, Pyrene, etc.

The oxygenated components remain on the column, and for this work, the

silica gel. in the column is discarded without further treatment.

G-l
-

The neutral or P.N.A. fraction obtained from the present analytical flow

, diagram for P.N.A. determination often exceeds the a l l owabLe limit for

P.N.,A.'s in the waste. Thus, the generator is required by law to treat

the material as a hazardous waste even though the analyst knows the fraction is in large part naphthalene or ot her neutral P.N.A.'s not of concern

as toxic components. To save the generator from unnecessary hazardous

waste handling expense when this situation occurs, the P.N.A. fraction

should be analyzed using EPA method 610 (quantitative high pressure liquid

chromatograph) or an equivalent method. These components are then subtracted from the weight of the P.N.A. fraction before the percent of P.N.A.

in the sample is calculated.

G-2
'----,

APPENDIX G

FIGURE 1

POLYCYCLIC AROMATIC HYDROCARBON (P.A.H.) ANALYSIS

STOCK PET. ETHER

FRACTION NO.1

I

Extrec:t twice with 1 vol.

of2NHC1 ••ch

PET. ETHER FRACTION

Extract twice with 1 vol

of 2 N NeOH uch

NaOH SOL. PET. ETHER FRACTION No.4

ACIDIC GROUPS NEUTRAL GROUPS

DISCARD

I

Evaporate end weigh

If) 1% dissolve in

pet. ether and chromet. on

activated lilica gel column.

(see text)

HC1 SOL.

BASIC GROUP

DISCARD

Elute with 5

column vol. of

pet. ether

•

ALPHATIC GROUPS

DISCARD

Elute with 3

column vol. of

benzene

+

P.A.H. FRACTION No.6

II

EVAPORATE & WEIGH

(see text)

HIGH PRESSURE LIQUID

CHROMATOGRAPHY TO

DETERMINE SPECIFIC

POLYCYCLICS OTHER THAN

4,5 or 6 RINGED (OPTIONAL)

G-3

COLUMN CONTAINS

OXYGENATED GROUPS

DISCARD COl. CONTENTS
.:)

APPENDIX G

ATTACHMENT 1

Preparation of a silica gel. chromatographic column:

A. Activated silica gel - 100/200 mesh silica gel (Davison Chemical

Grade 923 or equivalent) is a~tivated by heating in an oven at

1300 C. for 16 hours.

B. Chromatographic column - 300 mm. long x 10 mm. 1.0. with course

fritted disc at the bottom and a teflon stopcock.

C. Packing column - prepare a slurry of activated silica gel. in pet.

ether in an amount that will fill the column by about two thirds

after gentle tapping to settle the silica gel. Add 1 - 2 em of

anhydrous Na2S04 to the top of the column. Flush the column

with one column vol. of pet. ether. (Column volume - vol. in the

column occupied by column packing.)

Caution: Do not let the liquid drop below the packing in the column. LO

do so would trap air in the column and change its chroma tograph~c characteristics•

G-4