# ..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. Ignitability 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. Ignitability Corrosivity Reactivity EP Toxidty 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



## r-: G-l**--.~'** 

### 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 ignitability, corrosivity, reactivity, and extraction procedure (EP) toxicity. 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 characteristics, reactivity 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 1400 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.)

-1-2. .---.

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

-2-.---... 

# .-,

.....>



### 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.



### -3-••••• 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•

-5-

# n**"~~;;,.**..... :/**r'.~'~** -::;: 

## '0' APPENDIX

-6-**:~**
..}
•.•**~;** ... r

...**..:7:~·**...**~}** I: 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;**'.~."d' f"~~~\** **.,,:~;-j** 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 Oxidizcr: defini! iun.

An o xidizvr for the purpose- uf lbi.s suncnapu-r is a substance xuch a.:; :, chtoratc. pcrruauganatc. inorgnntc p.-r oxide, or a nitratc. 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 RIi:L!.'>1a Oq:ani

.. peruxid

..: d..finition,

(a) An orn.uuc compound cont.a.ining the uivalcut -0-- 0- structun- and which may be considered a derivat.ive 'of hydrouun peroxide where OlW or mor« of the hydrogeu atoms hav« bCl:n rep lacvd by on.:ani" rudicals must be classed as an orgnuic peroxide unless:

(1) The mut.r-ria l meets the dofinilion of all c xplu-avc- A or exptosiv« II, as prc,:cribeu ill Subpart C of this part, in which cas" it must bl' classed as an exploxiv«.

(2) Till' materi.u is Iorbiddun to OL' orr·:red for trruisport.auon uccorduu: u. § 17:!,101 or 1';:3,:!1 of this subchapter,

(3) It is dc-tcrrntncd that the predornin.uu, 1Iaz:,n1 uf t hc mntcrlnl CUll**l:tillitl~** all urg'l-nit, pcroxide is other than that of all oruanic peroxide. or

(-1) Accordiiu; tll data on file with tlu- Mntcrinlx Trunxuortntion Bureau, it l::lS bee-n clctcrnuricd i luu, th" m atcrial docs not pn's,'lIl a nazard ill tr.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~ ~:.!.**  tBSu:

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, reductants 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.**·.~,**

. ,"
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 instzucttons, 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

### J 

### ",



# (

'-./ I .,........,,\

_. J 

### 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 • thickness, D • diaalet 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 

### L

8.
- 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 I ... 

# - _.'. ·On**Re~~sioD** 

### A 8/8/80 

# -...

# .. 

# "--_.-

....

# ---..-_-------_._--**/~**

,

# (:

.... ;

, - . I"

..... ,.. •


# ... 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



# ..

# -

# ,-

.... _ .. .... __ -........ 4 _: ...... _ ••

__ ...... -*"

__ .....**_~** ......... _ .. , ,-... "- ....

# _.-
.. .... 

### - 

### -- 

# --

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/cm2 

### (129 amp/in2) 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 environment
. 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 tnll1sportal ion of tlH' fo llowiug c xptosivcs ,s Iorniddcn:

(n.) Explosive compounds. mixtures or devices which ignite .-;pon(:uwously or undergo rnark r d dr-compostt.iou when subjectr-d to a \C'lnjWratllf(' of 167" F. (7.')' C.) for 41\ consr-cut iv. hours.

(b) New explosive compounds, mixtures or devices except**a.~** provided tor in § 173,86,

(c) Explosive mixturr-s or devir-cs containing an arnrnorrium salt. nnd :1 chlorate. <d) Exnlosive mix! ures or r!P\"ic,'" coritai nlug an acidic mr-tal sa.lt and :t chlorrur-.

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

(f) Nit.rozlvr-erin. rli,·th.\'\f'IH'**t:I~'(',,1** din itrn.tc or otlu-r li(l'lid n;lliosin's Ilnl authorized hy H7,l,S:H"j or th i. (Fl'r shipmr-nt by motor vr-hir-lr- ot h.-r Ilt;\:\ by common cnr riur, :;",,' 177,8::2( lJ\ nr this subrhapt.r-r.j

(g) Loadr-d firearms. (h) Fireworks t.hnt ('o:nbilll' an ('Xplosivr- and a dr-tonn ror or h\a!:tilll\ cap,

(i) Piruworks contnintru: yel\()\\' or whitc nhosnhorous.

(j) Toy torpedoes. \he maximum Ollt· sick dirru-nsion of wh ir-h pxcp.'ds ;•. inch, or t.oy I.orp'.'d.,(,s coutainuu; 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, "'lInDosilio u ill each torpvr!o**{'xc{'l'din~:** four f{rain:.:.

C-6**~'\**

....-.**,,~**

## ~~**,,_.~** .. 11173.53**n,~finitinn** of class ,\ explnsivcs. (a) Type 1. Solid cxnloslvcs 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.ing cap (.'iee Note 2). Example: Black powder and low explosives.

(b) Tvpc 2. Solid cxplostvcs 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** blasting 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 ex pioded in rnorrthan 50 percent of ! he trials under a drop of less than 4 inches. Example: High explosives. commercial dynamite containing a liquid explosive ingredient.

(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 tlie trials under a drop of less than 4 inches. Example: High explosives, cornuu-rciat dynamite contairiing no liquid explosive ingredient, trinitrotoluene, amatol. tctryt. picric acid, urea nitrate. pcruolite. and commercial boosters,

(d) Type 4, Solid cxplostvc-s which can be caused to uetonate when unconfined (see Note 3). by contact .vith sparks or flame such as nroducr-d by safvty 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 prim**in~** explosives. kad**a;~idl'.** Iulm matc of mercury, et.c., uud**hi~h** «xplosivvs.

ie) Type 5. l)t-s('nsil :'·.,·d liquid ex p lo- :;i\'t'S are expl"s:\'t:,; whicl: rnay bt' detunated scparutrly or \\'I1I'n :tbsorl)l·d in suril«**allSllr~)L'llt** covtcn. 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,; signilit'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~lY** j'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-tal or plaxt.ic casiru, c:.>nl:lil:;:.;.; initiatnu.. or pr:nlillf,: ('Xp!usi';es.**('::l.~S** :\

.. 1'YPI' -t. l'IUll'r witl: or \I'd ::u\i'. othcr cxplosivcs. It is al'tiL':tll'd by .u:v cne of several**rnt'~1I1S,** illl'luding a:1 l·!-'clri· cal pulx«, it flanlt·. a snock or detonation wa\'t', rnechanical impart (percussion) pr;'ssuriz"d ga.s. or lIigll .nrenstt.y ligllt Iwam. It proudc,'S an ,'x;)]osive output that. may be used to initiate anothcr explosive or to perform work. A time delay may be im-orporan-d in t.he means of applying the st irnulus. or in the initialing device- itself'.

(1) A di-ton.uur (se(' Not." .1) is all initiating di-vico vother than on,' prop...rIy describ,'(\**:1..~** a dcton.u :!Or: fuze) which contains no more Ulan 10**~:r:(/l1:;** of total explosivcs**weigl)~** .•**'xcilldin~ i~nition**  and delay 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 wnict: art' percussion activated.

(iii) Blasting caps which arc act.ivatI'd by rkxiule**dctlln:Lt!Il~:** V'J: d. iurlud**ill~** .-

(:\) Delay connector.. in plast.ic slll'",llS which consist of**~l** plastic skL'\'e that. contains a suit.able delay syxtcn: will) n'('('ptnr and .tor.or explostvc**char~('s** in till' ("'Iller portion.**l~adl** l'lId Ill' Ihe sh-cvc I.; l::ack so that fli-xib le d.·tflllaling curd (';t:l be insertt'd lille) und Iockr-d to t:I<.· ('I,nll,'ctor:

I 131 Delav 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· tiUll 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';1iJ:, 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 cxploslv«**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, renr-t.ion.

( v ) Bla,stil1f; c,ap:; whirl: ar«: :lei i',"I.:I'<! by a shock tube,

(vi) Elcrtr ic blast.inz cap"**',I'~ljl'll** arractivated bv all electric' curront.

(2) A detonating primer (Sf'(' NOI" til is an initiation n('vice for commcrrinl use which contains more t.ha n 10 grams of total explosives wein 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-tonate 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** explosive. such as tctryl or dry rut.rocollulose. 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 th ey will not cause functioning of other fuzes, cxploxives, 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 whirh 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 cxplosivc projf'('t ilr«, "::1" :'rq.if"" i 1}' .:.**~n1()kp ;)roj(~(':**  iit s.,**~tll·i'ndi:l.r:: ;)r"~'('r'l**  ilex. ;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::;1 itu: 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 IIr. ')r D,,[ense (POD' and in accordance wi th r-stnbli::!ll'd pr:l"1 jet'S and I'r\H't'dlll'ls sp",'i, fi('(1 hy DOD,

'.k) Ernlosir» nroicctilrs. F>;pl"":I'" prn.i!'ctilf's arc sIll' II::, project,lt's, WOU'- ilC·:l.d:;, or rockr-!.**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': ar.: or O( II"r firing or launching dr-virr:'.

,.J) Grcuad cs. Gn'l1arft's, hanel or ri Ile, arc small metal or ot hr-r containr rs dcsirmed I () be tIHo'.':11**h~:** hand or pnJj('cl.cd from a rifle, Til,')'**:l.J'(~** fill ..d with an explosivr- or a. liquid. ga.." or xo l id matcrtat surh :'IS :l. to x ic or tP:'IT r::lS or an inr-cndiarv or :'l11ok,' p rorluciflr:; rnatcrial and a bur:« 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. Exnlosivc bornhs arc 1I11'tai or other coni niners**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-pth 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(e

### C-8**.,~~** .

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

.**~-":' .~** 
. ". ; 

## ""-"' ly assembled or rnuy be shipr"J un.issembled in one outxid« com.aim-r.

tq) A IIIIlL 101u to i, .Ivf SIHu!l arIHs IL'iUt exulosiue prOj('t'ill.-s (II" i-icen dia rv proiectiles. Ammunit ion for slllall arms with explosive projvctiles and ammunition for small arms with inccndiary projectilr-s is Iixcd ammuniLion of caliber 20 mill imetus to be us-d in machine guns or c.umuns. and consists of a metallic canridge case, Llll' urimcr and the propelling ctiargu. with ex p losive projectile or inccndiary proivctile with or without dc-tonnt.ing ftlzP: tlw component parts necessarv for one firing being all in one assernbly. Detonating fuzes. trncc-r Iuzr-s. explosive or ignition devices or fuze parts wiLh explosives contained thercrn 111ust not beassembled in anuuunitiou 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. bornus, J.(l'l'lIac!<'s, ctc., load,'l\ with toxic, tear. 01' oth c r gas. smoke or incendiary aJ.('·l\t, abo such misccllaneous apparatus as cloud-gas r-yliudel'S. smoke gt'l\t'rat.ors, vt.c.. ui.u may be utilized to proj,'ct cncmicals.

ls) Booste rs. h u rstcrs, a.tid s upplc- 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.otor 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 ignitcr "'\'lth a thrust**pl~~tl'J ,~I~~!** **\s,·~th** a nO:::.'.!>:·{S):ll thr- ot lu-r ,,!,'!. ,':.":,'**r(',·~:('l** lilaLor carr ies It.:; own "·;!id u:-.:di;'.l·rrUt'l corubmat ion.) 'I'tn- jll'lliwllint-: ctmrge consists of a I11IXll.rt, .jj c1:':ll1icals :lnd.-'or cl\l'l11ical (;,HIl;)()Un,:s which \l, hen ign.Led is**('ap:_~i,'** ur burn, illli**!':lpic~ly** and produciru; rons.derable pr"ssurt' :1I1d which \\ ill xuxtain a dvt.onat.iun. Rocket motors. Cj:1SS A c xplosives,**,;l~ould** be nonpropvuxive in shipnu-ut (.St'C par:tgraph.s (l)C!) (il and tiil uf this sect.ion). Rocket mot.ors, class A explosivcs. 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». Ttu-y art' used to Pi'll!,"! and/or pl'u\'idt' th ruxt Ior gUidl'd ::lissi!es. rockt-tx. or xpacr-craft .

ti) A rod,t'l. motor to lJ(' l'l;nsidl.·rl'o "uonuropulsiv.-" must i)(' '::O;J:,!Jle of unrr-st.ruinc-d burniru, and ',\:11 not. ruove apprt'ciaLJly in uuv direction whcn ignitt:d by any mr-nns. Blast def1l:et.ors, thrust ncutruli.x-r.. or other shu ilur t!t'\'ict's must !J(' prrivi-n adc- 'luaU' by test. prior to au tlioriznt.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:: unchr ('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 tII:"**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 cxulostvc. Chan:,"1 nil well jet pr-rIorat ing guns m uxt 11'" !ll" trunsport.cd Wil11 blastirut 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 chcrnical mixtures which an'**C1o."·'I;:I<"~** to function bv**r;jpi(~** CO 11111ll:,Ii'II1 "f successive layers, lcc:wral!.v ,,\jill Ii: Il!' or nn smoke. The combustion is (·nl.· tr ollrd b,: composit.ion. sii''''. and fIll'::; of r:rain. Propellant cxploxivex. CllL';:, A. include some tri)l'S of .·;nlnkf'I,',';.' powder and some types of solid prilpl'l· lant explosives for jf't th 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

... tria l.. wlu-n tested in the pnckrurr-s in \\'11kll it is offnrcd for transport.at ion. ln condueling the test., one propr-Jlan; container shall be surrounded 

### uy hu-rt loaded containcrs of the same \','('j..:l1l

.. including 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 elect.ric squib placed within 0\ inches of the bottorn of the container, The pr.-sr-nr-r- of a crater and abse-nce of fl amI.' "llal1 \)f' considr-rcd a." evidences of dct.ouat.ion.

Non: 1: The dr-t.onnt.lon u-st is**lJ('rforJ~1C'd** by pladng Lll" samplr: ill nu opun-r-nd fib('r tube which Is SI'1. on the ('no of

### i' Ic-ad hl"rk npproximatr-ly**l'~** tnchr-s in diamr-tcr and 4 inches high which. In turn, is pla

....d ,," a solid base. A stf'l'1 pl:1.',(' may hI' p:ar,.,j ',1" tween tlll' fiber tnbr- and (he It'f,r1 hi"d:.

Non: 2: 1\ No. R I.'st bla.stillg' rap I' ('11' cont ainin,: \"\'0 grams of a nux: lire' of Bll P('f· cent rncrvu ry Iulmtuatc anti 20 prr(',':11 ;)1)' la

..

ssium ch lorate, or a Utp of 0qlJ:\:dt'r:l strvngt.h.

NOTE 3: "Uru-oru inr-d" as**\lSf't~** in I 11:.;:;**~;n"** t ion litH'S not t'\,'!uc1c tlu- u:...p l): a j':,;,"r**,~r** soft fib.:r lube

.....rapping 10 laci)it"I,';' '·t,;.

N0TF. 4: TI1I' Burr:);! of Explosivrs )!;)I1'''o,**ApP:lraltJ~4** i:; :l**tl'~tin,::** rlevin'**(k~il::',I',l** ..n 1.11:1.1. :l**~Ilidt'd** H·pound wcinht rl1a)' 11,- IIro\lp<'d Irom p1'l'cktf',n,inl'o lwiv.hl.,**~()** '1., to ill:p::ct spf'('ific**Qtlnnliti('~** of**11·1':i(~** or solid mat.r-rials unrlr-r fl Xl';! conditions. 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 gencrru Iunctlon by rapid combustion rather than detonation and include some explosive 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-oilh-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 asxomblcd ill O!\I' pil'c('. Fin', works must be in a finishnj st at». ,,:.:. elusive of !ll('rl' ornnm.-ntatlon. ;,,.:**.;~,;!.** plicd t.o thc' rdai! trade and mus: I),' ;;" const.rurted and packed tint. Ioo.« I'y. rotcclmic composition will 1I0t. b" 1'1"':'· "IIL in**p;1.('kaf~(.'s** in lransportat in11.

lr) .JC't. thrust u nitx r ja.t.o i. rla.';s II /'\. nlosivcs: ro.. -kot motors. rlaxs n '·:,I';tl· sivcs: igniters, kl ,Ilrusl tiato ).**";:~** '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 metat cylfndr-rs ('onl ainiru; a mixturc 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-rnplnnr-« to t:lkl' off.

.

(21 l{cwkl'll!lotor, rlnss B l':,<pIO":I\'-·;', is a d"vict' cont.ainiru; 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 icnlt.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:1rri,':; 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.utl1orization 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~** ancl SpacC' i\O!. ministratio'1.

C-ll ,:11 Jgllilt'rs, j"l thrust (jato), class B rxplosh'(':<, 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-.. ruotrlv controllcd il:ni: ion element :1,,(\ a' Iast hur-ninc 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: th- 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.** rlass B, are**so~id** or liquid chr-mtcats or chemical**l~lIX'** rurr-s which :llnetion by combust.ion. Tile comh:l.«! ion L.; r-ont.rnllud by cornpositinn, siz«. Iorrn of gr:1ill, or othcr chl'll1ical or rnor-hn.ntcnl means. Any propellan( is elass B which fails to dotnl1:,,(' in fh'r t.rinls when t.ost.ed (Sl'r 1'ott' :n in tlu- par:k:1gl' in which it is oCff'r('c! for slupmr-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 monupropcllunt fl1l'1 (.'>t'r. Note 3), smokctess powder. or solid propellant cxploxivr-s for rricket 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' ('jecting 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 Director 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 lh,' 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-tOll: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' Arrny , Navy, or .·\ir l··I.I"L·l' 01 liu-**l:~.i·.l'd St.~(I·.'"**  CiU',I'ITiiJH·IH.**:.~I:L::** l.it· rl..........l:: .t... a fla:r ..:nablt· sol id lor**pur~_hlsi'S** 0:**tr;111~;}On:t·** tion '.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.aininu a Pl'('s:<<:d vyl indrical block of propellant oxptosiv

.. · and havin., in th,' top uf tlucas", a smal! compnrtnunt tllat ill' close-s an ..lectrica! .';l;l:ib. small amounts of black powde-r. and s.nok« less powder. which CUI1<:lutcs all i>;, nite-r. TIll' startcr cartr:·h:c is u::,·,j to acuvau- a mccluuur-a:**,,1;lr~,'r** 1'1';- .Il'l erigiru-s.

(j) Rockct c'ng"ille tl lquid ). clnsx Is r-xplosin';; I:; a COlllpll'll'. St'!f,collcainl'd rocke-t propu1:.,:on uni[ wl1ich contuiIlS an nxidiZt'r and :1 fuel. each scuaratcd by an :t111I11i!1l1l1l or**~;I** :lillit'S:; 

### ;;t"", w.i ll of not I":i:'; thnn**O.~!)(J** illr:ll thickru-ss. D',lll,j(, walls aI'" 1H'r111 iItl'd. 1'[('ssur, iZ:lli(//1 of tile propr-Hant tanks 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 

### Msodium acetate/O.l 

### Macetic 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 solid phases as described under "Separation Procedure." 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 Lbed in "Methods for Analysis of Water and Wastes. ")
D-3APPENDIX 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-- 

# 1

Discard 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

:-....

.: ..".:

......,

9.0 

# 1 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 I

## nner 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 EXTRACTION 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 characterLstt cs for the organic material. (Example: CH2C12

- dfch Loromethane, ) 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 CH2 CI2 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. ScopeandApplication 1.1 This methodisapplicableto drinking, surface. andsalinewaters, domesticandindustrial wastes. 1.2 Themethodissuitableforall concentrationrangesofchloridecontent; however, 

### inorder to avoid large titration-volume, asamplealiquotcontainingnot.morethan 10 to 20 mg CI per 50

### m1 isused. 1.3 Automatedtitrationmay be used. 

### 2. SummaryofMethod 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 formationoftheblue-violetmercurydiphenylcarbazonecomplex. 

### 3. Comments 3.1 Anions and cations atconcentrations normally found in surface waters do notinterfere. 3.2 Sulfiteinterferencecan be eliminatedby oxidizing the 50 ml ofsample solution with0.5 to 1

### m1 ofH202 .

.4. Apparatus 4.1 Standardlaboratorytitrimetricequipmentincludinga I ml or5

### mlmicroburetwith0.01 

### 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) 

### inchloride-freewaterin a 1litervolumetricflask and diluteto themark. 

# 5.. Nitricacid, HN01solution(3 

## + 997) 5.3 Sodiumhydroxidesolution, NaOH, (10 gil) 5.4 Hydrogenperoxide(30%), H202 5.5 Hydroquinone solution (10 g/liter): Dissolve 1 g ofpurified hydroquinone in water

### in a 100mlvolumetricanddilutetothemark. 5.6 Mercuric nitrate titrant (0.141 N): Dissolve 25 g Hg(NO)2·H20 in 900 

### m1 ofdistilled 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 chloridesolution (5.1) using procedure6. Adjustto exactly 0.141 N andcheck. Storein a darkbottle. A 1.00 ml aliquotisequivalentto 5.00 mg ofchloride. 5.7 Mercuric nitrate titrant (0.025 N): Dissolve4.2830gHg(NOJ)2·H20 in 50 ml ofdistilled water acidified with 0.5 ml cone. HNOJ(sp. gr. 1.42) in a I liter volumetric flask and dilute to the markwith distilled water. Filter ifnecessary. Standardizeagainst 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 adarkbottle. 5.8 Mercuric nitrate titrant (0.0141 N): Dissolve 2.4200 g Hg(NO))2-H20 in 25 ml of distilled wateracidified with 0.25 ml of cone. HNO) (sp. gr. 1.42) in a 1litervolumetric flask and dilute to the mark with distilled water. Filterif necessary. Standardizeagainst standard sodium chloride solution (5.1) using procedure 6. Adjust to exactly 0.0141 N andcheck. Storein adarkbottle. A I mlaliquotisequivalentto 500 ugofchloride. 5.9 Mixed indicator reagent: Dissolve 0.5 g crystalline diphenylcarbazone and 0.05 g bromophenol blue powderin 75 ml 95% ethanol in a 100 ml volumetric flask and dilute to the markwith 95% ethanol. Storeinbrownbottle anddiscardafter6months. 5.10 Alphazurine indicator solution: Dissolve 0.005 g ofalphazurineblue-green dye in 95% ethanol or isopropanol in a 100 ml volumetric and dilute to themark with 95% ethanol orisopropanol. 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. Ifthe concentration is less than 2.5 mg/I ofchloride, use 0.0141 N mercuric nitrate titrant (5.8) in step 6.6, a I rnlor 5 ml microburet, and determine an indicatorblankon 50 ml chloride-free water using procedure 6.6. If the concentration is less than 0.1 mg/l of chlorideconcentratean appropriatevolume to 50 ml. 6.2· Add5 to 10dropsofmixed indicatorreagent(5.9), shakeorswirl solution. 6.3 Ifa blue-violet or red color appears add HNO) solution (5.2) dropwise until the color changesto yellow. 6.4 If a yellow or orangecolor forms immediately on addition ofthe mixed indicator, add NaOH solution (5.3) dropwise until the color changes to blue-violet; then add HNO) solution(5.2) dropwiseuntil the colorchangesto 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 oftitrant normality. Alphazurine indicator solution (5.10) may be added with the indicator to sharpen the end point. This will changecolorshades. Practiceruns shouldbe made. 6.7 Additionalstepstoeliminateparticularinterferences: 6.7.1 If

### chromateispresentat 

### < 100mg/l and iron is not present, addsomealphazurine indicatorsolution (5.10) andacidify to pH 3(indicatingpaper). Endpointwill 

### then be an olive-purplecolor. 6.7.2 Ifchromate is present at 

### > 100 mg/l and iron is not present, add 2 ml of fresh hydroquinonesolution(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 chromateion. Add 2 rnl freshhydroquinonesolution (5.5). 6.7.4 Ifsulfiteion ispresent, add0.5 rnl ofH10 2

### solution (5.4) to 50 rnlsample andmix for 1minute.

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 exactincrementsofchloride, with the following results:

(FWPCAMethodStudy I, Mineraland PhysicalAnalyses) 8.2 In a single laboratory (EMSL). using surface water samples at an average concentration of34 mgCVI, thestandarddeviationwas :t 1.0. 8.3 A syntheticunknown samplecontaining 241 mg/l chloride, 108 mg/l Ca, 82mg/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% andarelativeerrorof2.9%. 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 Fraction 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 other 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 chromato**graph~c** characteristics •

G-4