Item ID Number 00237

Author

Federal Supply Service, General Services Administratio

RopOrt/ArtidO TitlO Federal Specification: Herbicide: Silvex Ester, andSilvex Potassium Salt, 0-H-215a

Journal/Book Titlo

Year 1965

Month/Day Au9ust

Color Ll

Number of Images 15

UBSCriptOO NOtOS Found in a file Labeled: "Technical Manual-Use ofHerbicides + Federal Specifications for Herbicides";supercedes O-H-00215 (Navy-Docks)

Monday, January 22, 2001 Page 287 of 341

AT*-IO5a

usffK, 11965

Ijit. Fed. Spec. O-H-00215 (Navy-Docks)May 15,1964

FEDERAL SPECIFICATION

HEEBICIDE: SILVEX ESTER, AND SILVEXPOTASSIUM SALT

This specification was approved by the Commissioner, Federal Supply Serv-ice, General Services Administration, for the use of all Federal agencies.

1. SCOPE AND CLASSIFICATION

1.1 Scope. This specification covers threetypes of organic acid herbicides known asiSilvex which are formulated with 2- (2, 4,5-trichlorophenoxy) propionic acid, and in-ert ingredients^ as either a low volatile liq-uid ester, or as a liquid or granular potas-sium salt. The liquid ester, when emulsi-fied with water or an oil-water carrier, isused as a selective translocated foliarspray for the control of many broad-leavedweeds and some woody plants. The liquidor granular potassium salts are used forthe control of aquatic weeds by direct ap-plication to water surfaces. Further infor-mation on use is contained in section 6 ofthis specification.

1.2 Classification.

1.2.1 Types. The silvex herbicide shall beof the following types as specified (see 6.2):

Type I—Liquid ester formulation: 2- (2,4, 5-trichlorophenoxy) propionic acid,low volatile esters; (4 pounds acidequivalent per gallon concentration).

Type II—Liquid salt formulation: 2- (2,4, 5-trichlorophenoxy) propionic acid,potassium salt; (60 percent by weight,or 6 pounds acid equivalent per gallonconcentration).

Type III—Granular salt formulation: 2-(2, 4, 5-trichlorophenoxy) propionic ac-id, potassium salt; (22.8 percent by

weight, or 20 percent acid equivalentconcentration).

2. APPLICABLE SPECIFICATIONS,STANDARDS, AND OTHER PUBLICA-TIONS

2.1 Specifications and standards. The fol-lowing specifications and standards, of theissues in effect on date of invitation forbids or request for proposal, form a partof this specification to the extent specifiedherein.

Federal Specifications:

RR-S-366—Sieves, Standard for Test-ing Purposes.

PPP-C-96—Cans, Metal, 28 Gage andLighter.

PPP-D-705—Drum: Metal Shipping,Steel (Over 12 and under 55 Gal-lon).

PPP-D-723—Drums, Fiber.. PPP-D-729—Drums: Metal, 55-Gallon

(For Shipment of Noncorrosive Ma-terial).

PPP-P-704—Pails: Shipping, Steel (1Through 12 Gallon).

Federal Standards:

Fed. Std. No. 102—Preservation, Pack-aging, and Packing Levels.

Fed. Std. No. 123—Marking for Domes-tic Shipment (Civilian Agencies).

FSC 6840

O-H-215a

(Activities outside the Federal Government mayobtain copies of Federal Specifications, Standards,and Handbooks as outlined under General Informa-tion in the Index of Federal Specifications andStandards and at the prices indicated in the Index.The Index, which includes cumulative monthly sup-plements as issued, is for sale on a subscriptionbasis by the Superintendent of Documents, U. S.Government Printing Office, Washington, D. C.f20402.

(Single copies of this specification and otherproduct specifications required by activities outsidethe Federal Government for bidding purposes areavailable without charge at the General ServicesAdministration Regional Offices in Boston, NewYork, Washington, D. C., Atlanta, Chicago, KansasCity, Mo., Dallas, Denver, San Francisco, LosAngeles and Seattle, Wash.

(Federal Government activities may obtain copiesof Federal Specifications, Standards, and Hand-books and the Index of Federal Specifications andStandards from established distribution points intheir agencies.)

Military Stwdards:

MIL-STD-105—Sampling Proceduresand Tables for Inspection by Attri-butes.

MIL-STD-129—Marking for Shipmentand Storage.

(Copies of Military Specifications and Standardsrequired by contractors in connection with specificprocurement functions should be obtained from theprocuring activity or as directed by the contractingofficer.)

2.2 Other publications. The following pub-lications form a part of this specificationto the extent specified herein. Unless oth-erwise indicated, the issue in effect on dateof invitation for bids or request for propos-al shall apply.

Code of Federal Regulations:

7 CFR 362—Agriculture, Regulationsfor the Enforcement of the FederalInsecticide, Fungicide, and Rodenti-cide Act.

(Copies of the above part of the Code of FederalRegulations may be obtained from the Superin-tendent of Documents, U. S. Government PrintingOffice, Washington, D. C., 20402.)

American Society for Testing and Mate-rials (ASTM) Publications:

ASTM D 56-57—-Test for Flash Pointby Tag Closed Tester.

ASTM D 97-57—Test for Cloud andPour Points.

(Application for copies should be addressed tothe American Society for Testing and Materials,1916 Race Street, Philadelphia, Pa., 19103.)

3. REQIREMENTS

3.1 Type I—Liquid ester formulation.

3.1.1 Composition. The type I silvex esterherbicide shall be a low volatile liquid esterformulation that is readily miscible in die-sel oil, fuel oil, or kerosene, and is read-ily emulsifiable in water. The finishedherbicide shall be composed of such activeingredients, inert ingredients, carriers,emulsifying agents, and solvents as are spec-ified herein.

3.1.1.1 Active ingredient. The active in-gredient shall be a 2- (2, 4, 5-trichlorophen-oxy) propionie acid low volatile ester. Itshall be in the minimum concentration of4 pounds acid equivalent per gallon, whentested as specified in 4.5.1.1. The particularesters used in the formulation shall be thebutoxyethanol, iso-octyl, or propylene gly-col butyl ether esters, or other heavy molec-ular weight esters of 2- (2, 4, 5-trichloro-phenoxy) propionie acid that are of thelow volatile type. However, methyl, ethyl,propyl, esopropyl, butyl, amyl, and pentylesters or mixtures of these alkyl esters arenot acceptable.

3.1.1.2 Inert ingredients. The inert in-gredients shall include the related im-purities and such diluting, modifying, andconditioning agents as are needed to meetthe requirements of this' specification.

3.1.1.2.1 Carrier, The carrier of the for-mulation shall be an oil that has an aromaticcontent large enough to keep the emulsif ierand the ester homogeneous at low temper-atures but small enough to avoid contact

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action what would 'kill plant cells and tis-sues to the extent of inhibiting translocationwhen a water emulsion is used.

3.1.2 Volatility. The effect of the vaporsfrom the herbicide shall have an activityrating of 3 or less when tested as specifiedin 4.5.1.2.

3.1.3 Emulsion stability. The herbicideshall contain the necessary emulsifyingagents and solvents to form an emulsionwith hard or soft water such that, whentested as specified in 4.5.1.3, there shallbe no more th'an' slight creaming (0.7 ml.maximum) of the emulsion, and no apparentfree oil present. No aliphatic alcohol hav-ing two to five carbons in the chain shallbe used as solvents since such alcoholscould cause transesterification during pro-longed periods of storage. This requirementis intended to ensure that the emulsion willbe completely stable during the mixingand application period but will break soonafter reaching the plant surface.

3.1.4 Sedimentation. The herbicide shallbe a clear liquid containing not more than0.01 percent of sediment or crystalline sol-ids by volume when tested as specified in4.5.1.4.

3.1.5 Free add. The herbicide shall con-tain not more than 1.4 percent free acidwhen tested as specified in 4.5.1.5.

3.1.6 Flash point. The flash point (TagClosed Tester) of the herbicide shall benot less than 60°C., when tested as speci-fied in 4.5.1.6.

3.1.7 Pour point. The pour point of theherbicide shall be minus 23°C. or lower,when tested as specified in 4.5.1.7.

3.2 Type II—Liquid salt formulation.

3.2.1 Composition. The type II silvex po-tassium salt herbicide shall be a liquid po-tassium salt formulation composed of suchactive ingredients and inert ingredients asare specified herein.

Active ingredient. The active in-gredient shall be 2- (2, 4, 5-trichlorophen-oxy) propionic acid potassium salt. It shallbe in the concentration by weight of not lessthan 60 percent, and shall have a minimumof 6 pounds acid equivalent per gallon, whentested as specified in 4.5.2.1.

3.2.1.2 Inert ingredients. The inert in-gredients shall include the related impur-ities and such diluting, modifying, and con-ditioning agents as are needed to meet therequirements of this specification.

3.2.2 Reaction. The acidity of the herbi-cide shall be not greater than 2 percentcalculated as H2SO4 and the alkalinityshall be not greater than 2 percent calculat-ed as NaOH, when tested as specified in4.5.2.2.

3.2.3 Sedimentation. The herbicide shallbe a clear amber liquid containing not morethan 0.01 percent of sediment or crystallinesolids by volume when tested as specifiedin 4.5.2.3.

3.3 Type III—Granular salt formulation.

3.3.1 Composition. The type III silvex po-tassium salt herbicide shall be a granularpotassium salt formulation composed ofsuch active ingredients and inert ingredi-ents as are specified herein. It shall be arelatively free-flowing granular productwhich shall be dry, loose, nondusty, non-gritty, and free from foreign matter. Theherbicide shall be prepared by impregna-tion of an absorbent granular carrier witha solution of the active ingredient. The fin-ished herbicide shall be essentially in theform of dry granular aggregates. Beforebeing packaged, the final herbicide shall becured for a sufficient time after formula-tion to allow full absorption of the solutionof the active ingredient.

3.3.1.1 Active ingredient. The active in-gredient shall be 2- (2, 4, 5-trichlorophen-oxy) propionic acid potassium salt. It shallbe in the concentration by weight of not less

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than 22.8 percent, and shall have a mini-mum of 20 percent acid equivalent, whentested as specified in 4.5.3.1.

3.3.1.2 Inert ingredients. The inert in-gridients shall consist of j[l) fae granularcarrier, (2) the unevaporated solvent re-maining permanently as part of the dry fin-ished preparation, and (3) any impuritiesIn the active ingredient used in, preparationof the herbicide.

3.3.1.2.1 Carrier. The carrjer shall be agranular attapulgite clay or other mineralthat has the ability to hold and carry rel-atively large amounts of oily, waxy, or stickychemicals while retaining a dry and free-flowing condition in the finished herbicide.It shall be extruded (commonly designatedAA), and calcined (commonly designatedLVM). It shall produce a stable formulationwith the active ingredient either with orwithout a deactivqtor, and also have s.uf-fjcienlj absorptive capacity to inhibit agglo-meration, caking, and lumping.

3.3.2| Chemical stability. Not more than10 percent of the concentration of 2- (2, 4,54rich,lorophenoxy) propionic acid potas-siuip salt specified in 3.3.1.1 shall be lostfrom the herbicide when tested as speci-fied^ ip 4.5*3,2.

5.3.3 Reaction. The acidity of the herbi-cide shall be not greater than 2 percent cal-culated as H2S04 and the alkalinity shallbe not greater than 2 percent calculated asNaOH when tested as specified in 4.5.3.3.

8.3.4 Grain size distrib^ion.. The grainsize distribution of. the herbicide shall meetthe requirements in table I. The distribu-tion shall be determined by the dry sievetest specified in 4.5.3.4.

TABLE I. Grain size distribution (dry sieve)Sieve

Micron size2380590250

U. S. No.8

3060

Minimum99.8

Maximum

101.5

Percent passing

3.4 Labeling. The herbicides shall be reg-istered andl labeled in compliance with theFederal Insecticide, Fungicide, and Rodenti-cide Act. The following additional informa-tion shall also be included in the labeling:

Federal Stock No.Specification NoType

3.5 Workmajttghip. The herbicides shallbe free from any defects which would im-pair their intended use.

4. SAMPLING, INSPECTION, ANDTEST PROCEDURES

4.1 Unless otherwise specified in the con-tract or purchase ordfer, the supplier is re-sponsible for the performance of all inspec-tion requirements as specified herein. Ex-cept as otherwise specified, (the suppliermay utilize his own facilities or any com-mercial laboratory acceptable to the Gov-ernment. The Government reserves theright to perform any of the inspections setforth in the specification where such inspec-tions are deemed necessary to assure thatsupplies and services conform to prescribedrequirements.

4.2 Lot.

4.2.1 Herbicide, Foj- purposes of inspec-tion, a lot for each type of herbicide shallconsist of all herbicide produced by onemanufacturer under essentially the sameconditions and process, within the follow-ing limitations. In the event the herbicideis produced by a continuous^nm process, thelot shall contain herbicide produced ,in aperiod of not more than 24 hours. In theevent the herbicide is produced by a batchprocess, each batch shall constitute a lot. Ifthe herbicide cannot be identified to a par-ticular 24-hour period or to a particularbatch, all herbicide to be offered for deliv-ery at one time under a contract or ordershall be considered a lot.

4.2.2 Fitted containers. For purposes ofinspection, a lot of filled containers shall

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consist of all specified containers filled withone type of herbicide which are to be of-fered for delivery at one time under a con-tract or order.

4.3 Sampling.

4.3.1 Sampling for examination (type IIIonly) and for tests (all types of herbicide).When herbicide is sampled from a continu-ous-run process, three separate 1-quart or1-pound samples, as applicable, shall be tak-en from each inspection lot, and shall rep-resent, respectively, the first part, the mid-dle part, and the last part of the run whichconstituted the lot. When herbicide is sam-pled from a batch process, for type I andtype II herbicide one 1-quart sample shallbe taken from each batch and shall be rep-resentative of all portions of the batch; fortype III herbicide, three separate 1-poundsamples shall be taken at different locationswithin each batch. When herbicide is sam-pled from an inspection lot consisting of allherbicide to be offered for delivery at one14me, three separate 1-quart or 1-poundsamples, as applicable, shall be taken atrandom from the lot.

4.3.2 Sampling for examination of filledcontainers. A random sample of filled con-tainers shall be selected from each lot inaccordance with MIL-STD-105, at inspectionlevel I, and an AQL of 2,5 percent defec-tive.

4.4 Examination.

4.4.1 Herbicide (type HI only). Prior toconducting the tests specified in 4.5.3, thesamples of herbicide selected in accordancewith 4.3.1 shall be visually examined forconformance to the appearance require-ments of 3.3.1. If any one of the samplesfails to pass the examination, the lot rep-resented therein shall be rejected. Rejectedlots may be reexamined provided the man-ufacturer has corrected all defects. Themanufacturer shall furnish to the Govern-ment full particulars concerning the rejec-tion and the action taken to correct the de-fects.

4.4.2 FUl containers. Each sample filledcontainer selected in accordance with 4.3.2shall be examined for any defects of thecontainer and the container closure, forevidence of leakage, and for illegible, incor-rect, or missing marking. Each samplefilled container shall also be weighed to de-termine conformance to the quantity (netweight) requirement. Any filled containerhaving one or more defects shall be con-sidered a defective unit.

4.5 Tests. Samples of herbicides selectedin accordance with 4.3.1 shall be subjectedseparately to the tests specified herein asapplicable to each type of herbicide. If anyone of the samples fails to pass any one ofthe tests specified, the lot represented there-in shall be rejected. Rejected lots may bereinspected provided the manufacturer hascorrected all defects. The manufacturershall furnish to the Government full partic-ulars concerning the rejection and the ac-tion taken to correct the defects.

4.5.1 Type I—Liquid ester formulation.

4.5.1.1 Concentration of low volatile liq-uid ester of 2- (2, 4, 5>tricklorophenoxy)propionic add. Since an ester type wettingagent is present in the formulation, the es-ter content cannot be determined by saponi-fication. It is, therefore, calculated! fromthe amount of chlorine present. The sam-ple is decomposed by heating with sodiumperoxide in a closed bomb. The chlorinepresent is converted to inorganic chlorideand determined volumetrically by the Vol-hard procedure. A correction is made forany free acid initially present.

4.5.1.1.1 Reagents.

(a.) Sodium peroxide (Na202), reagentgrade. CAUTION: Na^Oa is both astrong caust!ic/ and an intense oxidizingagent. Nothing but glass or metal shouldcome in contact with the dry powder. If anyis spilled, use dry sand in sweeping up. Donot pour Na202 or any mixture containingNa2O2 into water, as it may ignite violently.

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(6) Nitric acid (HNO8). Dilute onevolume of reagent grade HN03 with anequal volume of water.

(c) Silver nitrate (AgNb3), 0.1 Nsta^dpd.j^ljiition^lDifsolvf 1M9 g. of rea-gent g/a(Je AgN03 in water and dilute to 1liter. ; Standardize the solution^ against re-crystallized potassium bromide!

(d) Ammonium thiocyanate (NH*-SCN), 0.1 N standard solution. Dissolve7.612 g. of reerystallized NH4SCN in wa-ter and dilute to 1 liter. Standardize the so-lution against 0.1 N AgN03 solution.

(e) Volhard indicator. Dissolve 100g. of ferric ammonium suffate in 15 ml. ofconcentrated HNO3 and enough water tomake 1 liter.

(/) Alcohol, 95 percent. FormulaSDA-30; 10 gallons methyl alcohol plus 100gallons ethyl alcohol,' or formula SDA-2B;1/2 gallon benzene or 1/2 gallon rubber hy-drocarbon solvent in 100 gallons ethyl * al-cohol.

(g) Sodium hydroxide "(NaOH) solu-tion, 0.1 N. Dilute a solution containing4.0 g. of low-carbonate NaOH to 1 literwith water and standardize against ben-zole acid as primary standard. Prepare astock solution of low-carbonate NaOH byfiltering or allowing the Na2CO8 to settlefrom a 48 percent to 50 percent solution ofreagent grade NaOH. Store in a polyethy-lene bottle.

, 4.5.1.1.2 Apparatus.

(a) Parr Sodium Peroxide Bomb, Ser-ies 2100, Flame Ignition Apparatus, 22 ml.This bomb consists of four parfs: (1) A 22ml. fusion cup, 36 percent or 94 percentnickel, 1-1/16 inch I. D. by 1-5/8 inch deepwith a 1/16-inch wall and a 7/16-inch bottom.(2) A nickel-plated brass body. (3) A nickel-plated brass cover fitted with a lead gasket.(4) A nickel-plated brass screw cap whichclamps the cup, body, and cover together.

(•&) Ignition housing plus a safety glassshield and safety glasses.

(.c) Blast lamp for air, gas, and oxy-gen.

(d) Gelatin capsule, No. 00.(e) Beckman model G. pH meter (or

its equivalent), equipped with a glass-calo-mel electrode system.

4.5.1.1.3 Procedure.

(a) Weigh about 0.4 g. of the herbicidesample in a gelatin capsule to the nearesttenth of a milligram.

(6) Add about 5 g. of Na202 to thefusion cup. Place the capsule in the cup, andcover with about 10 g. of Na202.

(c) Close the bomb, make sure thatthe lead gasket is in place, and tighten witha wrench. Place the bomb behind a safetyshield. Heat the bottom of the bomb forone minute with an air gais flame and thenwith the oxygen flame until it is cherryred (about 2 minutes). Allow the bomb toair-cool for several minutes and then coolto room temperature either by allowing thebomb to stand or by placing it under a wa-ter tap. Remove the screw cap, without dis-turbing the cover. Wash the outside of thebomb with distilled water.

(d) Remove the cover and wash anyadhering particles into a 600 ml. beakerwith 50 ml. of distilled water. Place the fu-sion cup in an upright position in the beak-er. Tip the cup over with a dry stirring rodand immediately cover the beaker with awatchglass. When the reaction has com-pletely subsided, remove the fusion cup witha glass stirring rod and wash thoroughlywith a stream of distilled water. If the cakehas not completely dissolved, return the fu-sion cup and heat the solution carefully un-til dissolution is complete. Cool to room tem-perature.

(e) Slowly neutralize the cool solutionwith dilute HN03 and add 5 ml. in excess.A very vigorous reaction, due to the liber-ation of excess oxygen, takes place at theneutral point or in the presence of excessacid. Avoid losses from this reaction. Add0.1 N AgNO3 in a measured excess of from2 to 5 ml. more than the calculated amountrequired. (The calculated amount of AgN03required will be approximately 50 times the

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sample weight in grams.) Heat to coagu-late the precipitated silver chloride and di-gest for 5 minutes.

(f) Filter the solution with suctionthrough a coarse filter paper, such as What-man No. 40, on a Buchner type porcelainfunnel into a 500 ml. pyrex filter flask witha side tube. Wash the beaker and precipi-tate in the funnel several times to removethe excess of AgN08. Cool, add 5 to 10ml. of Volhard indicator, and titrate the ex-cess AgN08 with 0.1 N NH4SCN to thefirst permanent reddish-orange end point.

(g) Run a reagent blank by bombinga capsule containing peroxide and carryingit through the normal analytical procedure.Correct the AgN08 titration in paragraph(f) for the blank.

(h) Weigh 10 g. of the herbicide sam-ple into a 250 ml. beaker and add 100 ml.of alcohol. Titrate ,the free acid potentio-mefcrically with 0.1 'N NaOH to pH 7. Thecorrection for free acid initially present willbe:

ml. of 0.1 N NaOH X 310

X sample weight (paragraph (a))

This correction is also subtracted from theAgN03 titration in paragraph (f).Calculation;

(1) Percent 2-(2,4,5-trichlorophenoxy) propionioacid ester.

net ml. of 0.1 N AgN08 X X X 100Weight of aample

*** Percent acid ester

whereX = equivalent weight in grams of the

particular acid ester used in theformulation to 1 ml. of 0.1 N AgN08

(Example: Should the formulation be withpropylene glycol butyl etherester, the equivalent weight (X)would be 0.01355.)

(2) Percent acid equivalent.

Percent acid ester X

whereY = molecular weight of the particular

acid ester used in the formulation

(Example: Should the formulation be withpropylene glycol butyl etherester, the molecular weight (Y)would be 406-5.)

(3) Pounds per gallon acid equivalent.

Percent acid equivalent

269.5

Percent acid equivalent

100

X 8.33 X sp. gr. of herbicide

= Pounds per gallon of acid equivalent

The procedure for the determinationof the specific gravity of the herbicide at20°C. is as follows:Apparatw:

(a) Pycnometer, 25 ml. vacuum-wall.(b) Thermometer, calibrated in 0.1°

C., such as ASTM E 1-61.(c) Analytical balance having a sensi-

tivity of at least 1/10 milligram at full load.(d) Analytical weights, class S.

Procedure:(a) Clean the pycnometer with a satu-

rated solution of chromic acid in concentrat-ed sulfuric acid. Allow it to stand a fewhours, empty, and rinse well with distilledwater. Dry the empty pycnometer, usingacetone. Weigh and record as E. (Thisweighing must be in duplicate but need notbe repeated for each sample.)

(6) Standardization: Fill the pycno-meter with freshly boiled distilled waterthat has been sufficiently cooled so that,when the pycnometer is filled, the tempera-ture of the water will be 20° C. Insert theplug and wipe the plug and neck dry withfilter paper. Put the glass cap in place andweigh at once. Repeat this standardizationprocedure at least six times. Record theaverage weight as T. (This need not be re-peated for each sample.)

(c) Transfer 50 to 100 ml. of productto a clean 250-ml. Erlenmeyer flask. Adjustthe temperature of the sample so that,when the pycnometer is filled, the temper-ature of the sample will be 20° C. Fill the

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pycnometer, insert the plug, clean the out-side of the pycnometer, and wipe the plugand neck dry with filter paper. Put theglass cap in place and weigh at once. Recordthis weight as T'.Calculation:

T' - E = WT — E = W

thenW

= "Specific gravity of the herbicide at 20°C.in air

•IV-B—• of pycnometer and sample at 20°C.T = weight of pycnometer and water at 20°C.E = weight of pycnometer.

W = weight of water at 20°C.W = weight of sample at 20°C.

4.5.1.2 Volatility: This test is a bioassayin which the..effect of yajxxrs on test plantsis observed. The relative vapor activity ofthe herbicide, can be desjgnaied numerical-ly. . '

4.5.1.2.1 Apparatus and materials.

:(a) Polyethylene containers, gastight,4 by 4 by 18 inches.

(&) 3-inch pots.(c) Whatman No. 1 filter paper, 9 cm.

in efiameter.(d) Pinto bean plants, about 4 inches

tall. ." 't ' ^ "(e) Ethyl alcohol, 95 percent.(/) 2- (i, 4, Vtrichloroprienoxy) p'ropi-

ohic acid (chemically pure)'.(0) .2-(2, 4, 5-tricMorophenoxy) propi-

opiQ acl4 butyl ester.• • • r • • •• " • • • • r .f

4.5.1.2.2 Procedure. ̂ Just .prior to testing,place a pot containing one growing beanplant in each polyethylene container. Dis-solve 2 mg. of the acid equivalent of theherbicide in 10 ml. of alcohol and thorough-ly moisten a filter paper by dipping in thesolution. Discard the container used in thisimpregnation. Allow the alcohol to evapo-rate, insert the impregnated filter paperinto the polyethylene container holding the

bean plant, and fasten 6 inches above theleaves. Seal the open end of the container.Place in a dark room maintained at 27° ±3°C. Following the same jprocedure, sub-stitute 2 mg. of the material in (f) for theherbicide as one control, and substitute 2mg. of the acid equivalent of the materialin (g) for the herbicide as the other control.Each test shall be repeated three times.

Condttsions:After 24 hours, observe the effect of

the vapor on the plant and rate as follows:0—no visible effects — no vapor activ-

"y-1,2,3—plants recover with no reduc-

tion in growth, slight epinasty — very lowvapor activity.

4,5$—plants recover, moderate epinas-ty, moderate terminal bud inhibition andmoderate stem curvature — low to moder-ate vapor activity.

7,8,9—Severe injury, plant does not re-cover, pronounced epinasty, pronouncedstem curvature.— high vapor activity.

10—plant killed — very high vapor aotivity.

The materials in (f) and (g) are usedas standards. The former is rated 0 and thelatter is rated 9.

To be designated as low volatile, anester must have a vapor activity rating of3 or less.

4.5.1.3 Emulsion, stability. One percent(by volume) samples of herbicide in waterof known hardness are agitated mechani-cally under controlled conditions. The emul-sions formed are immediately transferredto an ASTM long-form centrifuge tube andexamined at the end of 30 minutes for thedegree of creaming and for presence of freeoil.

4.5.1.3.1 Reagents. Use three types of wa-ter for these tests.

(1) Standard hard water, haviing atotal hardness equivalent to 342 p.p.m. ofcalcium carbonate. It is made by dissolvingthe following salts in distilled water:

8

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Calcium chloride, anhydrous 0.304 gramMagnesium chloride hexahydrate ..0.139 gramDistilled water to make 1 liter

(2) Average water, having a totalhardness equivalent to 115 p.p.m. of cal-cium carbonate. Mix one volume of hardwater with two volumes of distilled water.This concentration represents the greatestdegree of hardness expected from munici-pal water-treating systems.

(3) Soft water, having a total hard-ness equivalent to 35 p.p.m. of calcium car-bonate. Mix one volume of hard water withnine volumes of distilled water. This con-ictentration represents a reasonable valuefor falling rainwater and could be assumedto represent average cistern water.

4.5.1.3.2 Apparatus.

(a) Eberbach Varible Speed Me-chanical Shaker No. 5109.

(6) Bottles, round jar with metal screwcap and aluminum foil liners, 8-ounce size,approximately 2 by 5-1/8 inches.

(c) Centrifuge tubes, ASTM long formtype, 106 ml. capacity.

(d) Ceritrifug'e lube rack.':(e)"Lamp, microscope substage with

15-watt "bulb ancl daylight glass filter.(/) Syringe, 2 ml. capacity, Luer, re-

sistance glass.(g) Thermometer.

4.5.1.3.3 Procedure. Into an 8-oz. roundjar, pour 99 ml. of hard water at a tempera-ture of 18° to 24° C. By means of a 2 ml.glass syringe without needle, add 1 ml. ofthe herbicide sample to the water at therate of 1 ml. in 5 to 10 seconds.

Hold the outlet of the syringe 1 inchabove the water, surface and direct the flowof the^ concentrate towards the center(away from the side) of the jar. Cap thejar immediately. Invert and right the jaronce and observe for dispersibility.

Immediately place the test jar anddispersed emulsion on a mechanical shak-

er with the long dimension of the jar par-allel to the direction of movement. Agitatefor 3 minutes at 2 cycles per second andwith a stroke travel of 1-1/4 inch of theshaker bed.

Pour the emulsion immediately intoa centrifuge tube supported in a rack.Conclusions:

Observe and record the condition of theemulsion at the end of 30 minutes, notingthe location and volume of any creaming orthe presence of free oil. Inspect the emul-sion by placing the microscope lamp behindthe centrifuge tube to be observed.

Note: Creaming is a well-defined layer of con-centrated emulsion occurring either at the top orbottom of the tube.

Repeat the procedure with average andsoft water.

Following each use, thoroughly cleanall jars, centrifuge tubes, etc., to removeall traces of emulsifier. Finally, rinse atleast three times with distilled water anddry in an oven at 105° C.

4.5.1.4 Sedimentation. Thoroughly shakethe herbicide sample in its container, turn-ing from top to bottom. Pour 100 ml. intoa 100-ml. graduated cylinder and allow tostand for 24 hours. The herbicide shall beobserved at the end of this period for evi-dence of sediment or crystalline solids, andthe percent determined.

4.5.1.5 Free acid. A procedure is givenfor the determination of the free acid as2-(2, 4, 5-trichlorophenoxy) propionic acidby titrating an alcoholic solution of theherbicide with 0.1 N sodium hydroxide.The end-point of the titration is determinedpotentometrieally.

4.5.1.5.1 Reaffents.(a) Sodium hydroxide (NaOH), stand-

ard 0.1 N solution. Dissolve 4 g. of sodiumhydroxide in distilled water and dilute to1 liter. Standardize against benzoic acid ofknown purity.

9

O-H-215a

(6) Alcohol, 95 percent. FormulaSDA-2B; 1/2-gallon benzene or 1/2-gallonrubber hydrocarbon solvent in 100 gallonsethyl alcohol.

4.5.1.5.2 Apparatus. Beckman, model G,pH meter (or its equivalent) equipped witha glass-calomel electrode system.

4.5.1.5.3 Procedure. Add ji ,10, g. sampleQf t^Q herbicide Jo 100,mlv,oj£ alcohol andtitrate the solutiqn potentiometricaliy to apH of 8.0 with 0.1 N NaOH.. , ! " ' • • ' ' : ' - . • ' : • • -

Calculation;ml. of NaOa X N X 0.2695 X 100

~ grams of sample

•• Percent free acid

4.5.1.6 Flash point. The flash point (TagClosed Tester) of the herbicide shall be de-termined in accordance with ASTM D 56-57.

4.54.7 Pour point. The pour point of theherbicide shall be determined in accordancewith ASTM D 97-57. ~v...'

4.5.2 Type II—Liquid salt formulation.' , : ': '* • • ' " ' > • • • • > . - ' : : : ' . ' '.;

4.5.2.1 Concentration of liquid potassiumsalt of 2-(2, 4, 5-trichlorpphenoxy) propi-onic a<$d. The sample is decomposed byheatipg with sodium peroxide in a closedbombj ^The chjprine present is converted toinorganic chloride and determined volumet-rically by the Volhard procedure. A correc-tion is made for any inorganic chloride ini-tially present.

4.5.2.1.1 KeagentB. The reagents are thesaj^e as those, specified in (a) through (e)in 4.5.1.1.1, and the following: Nitroben-zene, technical.

• • : • • • ' •:;. . .:'..> . . - • ' . J* : : • ' " . i ; <. i-;. '

4.5.2.1.2 Apparatus. The apparatus is thesame as that specified in (a) through (d)in 4.5.1.1.2.

of water and 5 ml. of dilute HN08. Add2 ml. of Volhard indicator. From a_biirette,add 1 ml. of standard 0.1 N NH4SCN. Ti-trate with standard 0.1 N AgN08 until thereddish color disappears and then add 2 ml.excess. Add about 2 ml. of nitrobenzene tothe flask and agitate thoroughly to coagu-late the precipitate. Titrate the excessAgN08 with 0.1 N NH4SCN to a red-brownend-point which persists for about 30 sec-onds. The correction for inorganic chlorideinitially present will be:

ml. of 0.1 N AgN08

X sample weight (paragraph (a))

This correction is also subtracted fromthe AgN08 titration in paragraph (f).

Calculation:'(1) Percent 2-(2,<i^-trichlorophenoxy) propionie

• acid liquid 'potassium salt.

The molecular weight of the acid po-tassium salt is 307.6 and the equivalentweight relative to chlorine is 102.5. Onemilliliter of 0.1 N AgN08 is equivalent to0.01025 g. of acid potassium salt.

net ml. of 0.1 N AgN08 X 0.01025 X 100weight of sample

= Percent liquid potassium salt

(2) Percent acid equivalent.

269.6Percent acid potassium salt X

4.5.2.1.3 Procedure. Procedures (a)through (g) are the same as in 4.5.1.1.3.

(h) Weigh 5 g. of the herbicide sam-ple into a 250-ml. beaker containing 100 ml.

307.6= Percent acid equivalent

(3) Pounds per gallon add equivalent.

Percent acid equivalentIQO "

X 8.38 X sp. gr. of herbicide

=• Pounds per gallon of acid equivalent

(The procedure for the determinationof the specific gravity of the herbicide at20°C. is given in 4.5.1.1.3.)

4.5.2.2 Reaction.

4.5.2.2.1 Acidity.

O-H-215a

4.5.2.2.1.1 Procedure. Weigh exactly 10g. of the herbicide sample and disperse in100 ml. of distilled water with stirring. Fil-ter and titrate the filtrate immediately with0.02 N sodium hydroxide (NaOH), usingmethyl red as indicator. Carry out a blankdetermination on 100 ml. distilled waterwith 0.02 N NaOH.

Calculation:Acidity as H2S04 (percent) = 0.0098 X (a — b)where a = vol. in ml of 0.02 N NaOH used for

* the sampleb = vol. in ml. of 0.02 N NaOH used for

the blank

Note: The blank may take the form of a smalltitre with 0.02 N HC1, in which case

Acidity as H2S04 (percent) = 0.0098 X (a + c)where a = vol. in ml. of 0.02 N NaOH used for

the sampler c =*= vol. in ml. of 0.02 N HC1 used for

the blankAlternatively, the end-point may be determined

velectrometrically.

4.5.2.2.2 Alkalinity.

4.5.2.2.2.1 'Procedure. Weigh exactly 10grains of the herbicide sample and dispersein 100 ml. of distilled water with stirring.Filter, and titrate the filtrate immediatelywith 0.02...N hydrochloric acid (HC1), usingmethyl red as indicator. Carry out a blankdetermination in 100 ml. of distilled waterWith 0.02 N NaOH.

Calculation:Alkalinity as NaOH (percent) = 0.008 X (d + e)where d = vol. in ml. of 0.02 N HC1 used for

the samplee = vol. in mil. of 0.02 N NaOH used for

the blank

Note: The blank may take the form of a smalltitre with 0.02 N HC1, in which case

, Alkalinity as NaOH (percent) = 0.008 X (d — f)where d — vol. in ml. of 0.02 N HC1 used for

the samplef — vol. in ml. of 0.02 N HC1 used for

the blankAlternatively, the end-point may be determined

electrometrically.

. , 4.5.2.3 Sedimentation. The sedimentation

test is the same as that specified for thetype I herbicide in 4.5.1.4.

4.5.3 Type HI—Granular salt formulation.

4.5.3.1 Concentration of granular potas-sium salt of 2-(2, 4, 5-trichlorophenoxy)propionie acid. The sample is decomposed byheating with sodium peroxide in a closedbomb. The chlorine present is converted toinorganic chloride and determined volumet-rically by the Volhard procedure. A correc-tion is made for any inorganic chloride in-tially present.

4.5.3.1.1 Reagents. The reagents are thesame as those specified in (a) through (e)in 4.5.1.1.1, and the following: Nitroben-zene, technical.

4.5.3.1.2 Apparatus. The apparatus is thesame as that specified in (a) through (d)in 4.5.1.1.2.

4.5.3.1.3 Procedure.(a) Grind several portions of the herb-

icide sample to a fine powder with a mor-tar and pestle or micropulverizer, to makea total of 20 to 30 <s. Weigh about 1 to 1.5g. of the herbicide sample in a gelatin cap-sule to the nearest tenth of a milligram.

Procedures (b) through (g) are thesame as in 4.5.1.1.3.

(h) Weigh 15 g. of the herbicide sam-ple into a 250 ml. beaker containing 100 ml.of water and 5 ml. of dilute HN08. Add2 ml. of Volhard indicator. From a burette,add 1 ml. of standard 0.1 N NH4SCN. Ti-trate with standard 0.1 N AgN03 until thereddish color disappears and then add 2 ml.excess. Add about 2 ml. of nitrobenzene tothe flask and agitate thoroughly to coagu-late the precipitate. Titrate the excessAgN08 with 0.12V NH4SCN to a red-brownend-point which persists for about 30 sec-onds. The correction for inorganic chlorideinitially present will be:

ml. of 0.1 N AgN08

16X sample weight (paragraph (a))

11

0-H-215a

This correction is also subtracted from theAgNOs titration in paragraph (f).

Calculation:

(1) Percent 2-{2,4,5-triehlorophenoxy) propionicaci$ granular potassium, salt,

The molecular weight of the acid po-tassium salt is 307.6 and the equivalentweight relative to chlorine,is. 10.2.5. One mil-liliter of 6.1 ti AgN03 is, equivalent to0.01205 gram of acid potassium salt.

net ml. of 0.1 # AgN03 X 0.01025 X 100weight of sample

*= Percent granular potassium salt

(2) Percent acid equivalent.

Percent acid potassium salt X269.5807.6

•* Percent acid equivalent

4.5.3.2 Chemical stability. This test is in-tended for the determination of any chem-ical breakdown of the granular herbicidewhen stored at high temperature.

4.5.3.2.1 Apparatus.

(a) Oven, regulated to maintain 55° ±S°C.

(b) Storage jars, glass, approximately00 to 120 ml. with screw-caps and aluminuminserts in caps.

4.5.3.2.2 Procedure.

Load a clean dry storage jar approxi-mately half full of the herbicide samplewithout compaction. Close the jar tightlywith the aluminum-insert cap, and store inthe oven at 55° ± 3°C. fyr ;14 days.

. . . • ' , • . 'S .•• ' a -•£ '

Remove ̂ he jar from the oven and coolto room temperature, "fumble the sampleIn the jar to redistribute the dust uniform-ly among the granules, weigh out a 1.0 g.sample, and analyze for potassium salt asdescribed in 4.5.3.1. Calculate the loss, ifany, in percent of potassium salt originallypresent.

4.5.3.3 Reaction. The reaction test is the

same as that specified for the type II herb-icide in 4.5.2.2, except that dispersion in thedistilled water shall be accomplished byfrequent stirring for 1/2 hour.

4.5.3.4 Grain size distribution.

4.5.3.4.1 Sieves. Sieves used in this testshall conform to RR-S-366. Mesh sizes are2380-micron (U.S. No. 8), 590-micron (U.S.No. 30), and 250^-micron (U.S. No. 60). Sieveframe is 8-inch diameter, either full height(inside depth 2 inches) or half height (in-side depth 1 inch).

4.5.3.4.2 Sample preparation. Each timeany portion is removed from the stock sam-ple, extreme care must be taken to includethe proportionate amount of dust with thegranules, in order that both the withdrawnsample and the remaining stock be repre-sentative in dust content. This necessity isthe basis for the following procedure, to befollowed in every instance.

(a) Determine the weight of the stocksample.

(6) Tumble the stock sample end-ov-er-end at approximately 30 r.p.m. for 1minute in a jar whose volume is about twicethe apparent volume of the sample.

(c) Separate a 20<- to 25 g< portion asa test sample by turntable sampling as fol-lows: A sieve receiver pan, 8-inch diam-eter, 2-inch depth, is secured in a centeredposition on a 45 r.p.m. tumable (see 6.4).It is recommended that the drive mecha-nism for any speeds other than 45r.p.m. be inactivated to prevent their in-advertent use, A sheetTmetal receivercup, with plain thin unflanged rim isplaced within the pan. A 60° angle glassfunnel is adjusted on a support so that theoutlet tip just clears the top of the cup, andthe funnel and cup are set off-center withrespect to the turntable by such an amountthat the arc projected by the funnel tipacross the cup in rotation of the table willbear the same ratio to the complete circle

12

as the weight of tlie desired test samplebears to the weight of the whole stock sam-ple. The bore diameter of the funnel stemshould be just sufficient to provide freeflow for the granular material being treat-ed. With the turntable rotating at 45 r.p.m.,the entire stock sample is poured throughthe f unnerso as to be delivered continuous-ly in a steady stream*. In case of clogging orbridging, normal flow "is restored (the ta-ble still turning) by probing with a stoutwire flattened on the lower end. The por-tion for test falls in the cup, while the re-mainder falls in the pan outside the cup.The QUP is removed, any dust clinging totitle outside surfaces is brushed back intothe pan, and the cup with its load is weighedfor determination of the best sampleweight; the remainder in the pan is re*turned to the stock jar.

4.5.3.4.3 Procedure. Screen the test sam-ple through a nest of sieves of the desig-nated mesh sizes, using a single-eccentrictype mechanical shaker that imparts to thesieve a rotary motion and tapping action ofuniform speed of approximately 300 gyra-tions and approximately 150 taps per min-ute. Continue the screening for 15 minutes.Weigh the residues and calculate the per-centage passing through each sieve. In theweighing and transferring of the sieve sam-ple and its size fractions, any dust clingingto sieve cloth, sieve wall, scale pan and mis-cellaneous surfaces, or clogging the sieve-cloth apertures, is to be regarded as partof the finest fraction "(sieve-pan fraction).Neither this dust .nor the material actuallyentering the sieve pan need be recoveredfor weighing; the granules lying on the re-spective sieve cloths are to be recoveredand weighed, and the pan fraction calcu-lated by difference.

4.6 Inspection of preparation for delivery.The packaging, packing, and marking ofthe herbicides shall be inspected to deter-mine conformance to the requirements ofsection 5.

0rH-215a

5. PREPARATION FOR DELIVERY

(For civil agency use, the definitions andapplications of the levels of packaging andpacking shall be in accordance with Fed.Std. No. 102.)

5.1 Packaging. Packaging shall be levelA or C, as specified (see 6.2).

5.1.1 Level A.

5.1.1.1 Types I and II herbicides. Theherbicides shall be packaged in 5-gallontight-head metal pails conforming to PPP-P-704, type I, class 3; 30-gallon tight-headdrums conforming to PPP-D-705, type I;or 55-gallon nonremovable-cover metaldrums conforming to PPP-D-729, type II, asspecified (see 6.2).

5.1.1.2 Type HI herbicide. The herbicideshall be packaged in 1-pound, 5-pound, or10-pound quantities in metal cans conform-ing to PPP-C-96, type V, class 2, or in 50-pound quantities in fiber drums conformingto PPP-D-723, type III, grade A, as speci-fied (see 6.2) .

5.1.2 Level C. The herbicides shall bepackaged in accordance with the manufac-turer's standard practice. The size of con-tainers shall be as specified (see 6.2).

5.2 Packing. Packing shall be level A, B,or C, as specified (see 6.2).

5.2.1 Level A.

5.2.1.1 Types I and II herbicides. Theherbicides packaged in 5-gallon, 30-gallon,or 55-gallon metal containers as specified in5.1.1.1 require no overpacking.

5.2.1.2 Type III herbicide. The herbicidepackaged in 1-pound, 5-pound, or lO^poundmetal cans as specified in 5.1.1.2 shall bepacked in accordance with the overseas ship-ment requirements of the appendix to PPP-C-96. The herbicide packaged in 50-poundfiber drums as specified in 5.1.1.2 requiresno overpacking.

13

O-H-215a

5.2.2 Level B.

5.2.2.1 Types I and 11 herbicides. Not ap-plicable.

5.2.2.2 Type III herbicide. The herbicidepackaged in 1-pound, 5-pound, or 10-poundinetal cans as specified in 5.1.1.2 shall bepacked in accordance with the domesticshipment requirements of the appendix toPPP-C-96. The herbicide packaged in 50-pouiid fiber drums as specified in 5.1.1.2requires no overpacking.

5.2.3 Level C. The herbicides shall bepacked in a manner which will insure ar-rival at destination in satisfactory condi-tion and which will be acceptable to the car-rier at lowest rates. Containers and pack-ing shall comply with rules and regulationsof carriers .as applicable to the mode oftransportation.

i V ' - " ' .J : • : . " ' •

5..3 Marking.

5.3.1 Civil agendes. Interior packagesand shipping containers snail be marked inaccordance with Fed. Std. No. 123.

5.3.2 Military agencies. In addition to therequirements of 3.4 and to any special mark-ing required by the contract or order, in-terior packages and shipping containersshall be marked in accordance with MIL-STD-129.

6. NOTES

6.1 Intended use.

6.1.1 Type I. The type I silvex herbicidecovered by this specification is intended foruse in the selective control of many herba-ceous weeds and some woody plants grow-ing in pastures, rangelands, fence rows>ifight-of-ways, and ditchbanks. It is usedmuch the same way as '2, 4,' 5-T herbicideexcept that (1) it is safer'where drift ontocotton is a hazard, (2) it is more effectiveas a foliage spray on some oaks, maples,Salt cedar, redbud, cherokee rose, trumpetcreeper, trumpet vine, and yucca, (3) it isnot as effective for basal bark and cut sur-

face applications, and (4) it is more effec-tive on mouse-ear, chickweed, and henbit.

Susceptible species in addition to thoselisted above are: Blackjack oak, northernoaks (pin, red, white, scrub), post oak, sandshinnery oak, maples (red, sugar, big leaf),wild blackberry, black gum, cherry, elm,ground ivy, poison ivy, mesquite, broom-weed, cockleburr, cotton weed, curly indi-go, lamb's quarters, Mexican weed, poke-berry, ragweed, salt cedar, and sunflower.

Among the species hard to kill are:African rue, ash, hawthorn, hickory, mul-berry, Osage-orange, persimmon, pricklypear cactus, rabbit brush, red bay, redvine, multiflora rose, sagebrush, smilax,and sweet gum.

Buckbrush, coralberry, juniper, andwood's rose are resistant.

Although the type I silvex herbicide isintended primarily for use on land, it mayalso be used for aquatic weed control inponds and other still waters and is effec-tive against certain submergent weeds suchas fanwort, water milfoil, bladderwort, andwaterweed.

6.1.2 Types II and HI. The types II andIII silvex herbicides covered by this speci-fication are intended for use in the con-trol of a wide variety of submersed, float-ing, and emersed aquatic weeds in lakes andponds. They are less toxic than the esterformulations to fish. They do not injure landplants adjacent to treated areas. They aresimilar to 2,4-t) herbicide in their effect onmany species of submersed aquatic weedsand are more effective on some.

Susceptible weeds are: Arrowhead,coontail, naiad, fanwort, mule's ear, par-rotsfeather, pickerel weed, primrose willow,spatterdock, water hyacinth, water lilies,water milfoil, water plantain, water shield,water stargrass, and water starwort.

Bulrush, watercrowfoot, waterweed,duckweed, and some pondweeds are harderto kill.

14

6.2 Ordering data. Purchasers, should ex-ercise any desired options offered hereinand procurement documents should specifythe following:

(a) Title, number, and date of this speci-fication.

(&) Type of silvex herbicide required(see 1.2.1).

(c) Level of packaging and level of pack-ing required (see 5.1 and 5.2).

(d) Size of container (see 5.1.1 and5.1.2).

6.3 References for use in connection withthe active ingredient concentration tests(see 4.5.1, 4.5.2, and 4.5.3).

Parr Manual No. 121, Peroxide Bomb Ap-paratus and Methods, Parr InstrumentCompany, Moline, Illinois (1950). Parr,S.W., J. Am. Chem. Soc., 30; 764 (1908).Volhard, J.J., Pract. Chem., 9; 217 (1874).

6.4 Turntable. An approved turntable foruse in conducting the grain size distributiontest in 4.5.3.4 is the General Industries,

0-H-215a

Model TR, motorized 9-inch phonographturntable, or equivalent.

CUSTODIANS:

Army—MUNavy—YDAir Force—68

Review activities:

Army—MU, MO, MDNavy—YD, MSAir Force—68

User activities:

Army—SMNavy—MC

Preparing activity:Navy—YD

•ft U.S. GOVERNMENT PRINTING OFFICEl 196S—£03347/24

Copies of this specification may be purchased for 10 cents each.

15