---”’

.LA4JR -81-917

TITLE: EUTECTIC COMPOSITE EXPLOSIVES CONTAINING AMMONIUM NITWTE

AUTHOR(S): Mary M. Stineciph[~r

SUBMITTED TO: Yth Syml)osium (Int l.) on l)etond~ioll

Annapolis, M!)

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LOS ALAMOS SCIENTFIC LABORATORY

Post C)ltiGo 130x ICG3 Los A1OIINM, Nmw M[~xicu 87545
An Alflrmtive Actiow EqIKIl OL)p(vtwi?y h]~iuyor
r,
‘wt.’
 Pt. f! . st~ncelpher

EUTECTIC COMPOSITE EXPMSIVES CONTAINING AMHONIUM NITRATE!

M. M. Stinccipher
Iam Alarmo National Laboratory
Univ~rmlty of California
U3s,Alamos. New Mexico

ide have prepared, and mtudied ths sensitivity and

performance of, the eutectic of ammoniun n~trare
(*I and the a-nium salt of 3,5-dlnltro-
L,2,4-trlazolo. We found that this AN Formula-
tion was unumuaL in that it performed ideally at
small diameter, which indicated that it wna a
monomolecular exploalv~. Sensitivity tests in-
cluded type 12 impact, Henkln thermal snd wwdqe
testn, and performance tests included rate
ltlck/plate dent, cylinder, and aquarium Cesrs.
P,esulte were compared with calculation, st~ndard
explosives, and anuther ●utect~c, ethylenedLsm~nc
4initrate [EDD)/AN.

1. INTRODUCTION

?tonomalecular oxplos~ves arc.

limited in amount o! cnerqy that can
he buklt lnta rho mnlccule without it
beccm~nq too unstable to use. ll@w-
ever, if atl the oxyqen does not have
to be in the same molecule, a more
stable mmbination of oxidizer and
fuel-rich ●xploeivc can achieve the
~n?rqy of ● ~~-balsnced @mpLoIIivP.
Until recently, it had b-en thouqltt
(1) thet .s nolid solution -uld ht
necmassry for an l)xlrllxer find fuel to
Mhav= ●e one mmpound in th~ r!rtnna-
tion zon*, How*ver, experia-nt~ h-f
Vinqf?r (2) and co-@rk@re at Lawrencm
Livmrmore National Laboratory (LML)
sh-~rl that when th~ ~rt~cLe at-e 0[
tho oxldLzer was less than !3 ~m (ear
●xsmplv, ● a~slte of qtound parti-
CIQS of ammonium IWrc!rlorata eusp~nded
in y-lld nltromothan~) thmn th~ OXL-
dizmr reacts mmpl?tely ~n the d@tona-
tlon xono, am ~huw.1 by the ncallnq he-
t,ween 2.54- and 5, L!d-cm-dlaa cylinder
teste. McGuIre ;)) found thst i.wi~
topic nlmlnq r!vrinq d~tonatlon in a
monrnaml~ular osplomiv~ was random.
Eut.in the cane of a compmltm, Alatal
~]>.~~b~l~d a~~n~u. ft~tratQ (A~)/.
L j the isotoro ratio in th~ productm
lndicfitmd that only a 0.6 .m ltty-r of
t%! A!4 partlclem @3m1317WI with the
 M. H. S?inecipher

two roles of AN per male of ADNT to be Drierite in vacuum gave pure ADNT [35
~2-balanced. Because the C02- g, 0.2 mol. 67t yield) with a melting
forraulation wan not far Cron eutectic point Of 168-170°C. The yield waa
formlatlon, 1.38/1 wlar ratio AN/- improved by a second ●xtraction of the
ADm, all of the AN could be dissolved aqueous reaction ❑ ixture. ADW forms
in the eutectic melt by heating to a dihydrate at relative humidities
123% (7). We have studied the per- over 35t. The aminefr used war? terti-
formance of the ●utactic and 2/1 molar ary amines: Alamines 304 and 336
r~tlo M/ADNT, compared these results (General Hill Chemicals, Inc.) and ●
with calcul~ted resultn and compared secondary aminer Amberlite (Rohm and
our reaulte with those Akst has ob- Iiaas Co.). The mlar amunt of amine
tained Cor ●utectlc ED2VAN (6). umcd wan ●qual to the amount 02 the
DNT in the solution as measured by uv
11. MATERIAL FREPARATION upectrosc~py. The regenerated amine
eolution was reused after washinq with
Preparation of AD~ water.

We have modified the method of Preparation of Amine Sitrates

preparation of ADNT reported by the
Soviets (9), es~-ially the ❑ethod of we prepared EDD ~nd other ali-
isolation. The following is a sample phatic amine n~trates by dissolving
syrthesia and isolation. the a.~ine in 10S aqueoua ■ethanol and
adding :0/50 by volume concencraced
A nolution of 3,5-dl.lmlno- nitric acid/water tiropwtse while
1#2,4,- triazole (Aldrich) (30.0 q, coolinq with an ice bath to keep the
0.1 -1) in 0.68 !4 sulfuric acid (1.1 temperature sc ambient or below. Af-
{, L.5 ❑ol H+) was added dropwlse ter ne,Jtrsllzation wss complete, the
over 3 hours to a solution of sodium prc:lpttaced nitrate ~~lt wss fll-
nitrite (200 q, 2.9 mol.) in water (200 t~rod, w~shed well with methanol, tnrl
❑ll while keepif;n th~ reaction mixture recry~talllzed from water;metn~nol.
at 0% with an alcohol-lee bath.
Act?r addition was compl=c?, the re-
action wan heated to 600c and waa
held there for one hour until a~l pre-
-. cipitate had dlsaolved. Then the
reaction mixture was cooLed again to
0%, and acidified with 6 H suLfuric
acid (1OIJ ml, 1.2 mol H+). Thin
step converted the excess nod\um ni-
trite tm nitroum acid. urea (15 q,
0.25 moll wsm adtlad slowly (foamLnql
to romve any rema~ninq oxidas of ni-
troqen from solution. The completed
reaction mixture had a small amunt of
oranqe pr-clpltace chat wan removed by
●ddition of rlecolorkzirq carbn and
(lltratlon. Analysis of the filtrate
by ultraviolet npeckraecupy at 285 nm
snowed a 909 yield of l,5-dLnltro-
1,2,4-tria’tole (D~).
111. TESTING ,WIIODS
ThQ stronqly tcidlc character of
DW 1-0.66 pRJ) (10) ●ad- ●xtractiori Sannitlv19y
-- W9ta
—.
with tho usual orqanic aolventrn impo~-
slble. It can be ●retracted by the Miatureo *re tested lor saf~ty
continuwrm ■ethod with ●th’~1 ●ther, by findinq impact and thermal senaitb-
but tho flamabillty of ●ther ud~ vltles. Th@ wedqe t~at qave add~-
●nether method neceesary for larqe- tional ~nformatlon on ~nttlatlon.
scale r~actlona. We found that a
toluero ●olutlon (20t) of water- Impact e~noitlvity wan found on
lncol’Jbl@ m?condary or tertiary amlnea an ZRL-type machine ●q’Jlpp@d with typQ
Qatrscted the DNT from the ●queout 12 tmlo and a microphone for ooJnd
reaction mlxturc (11). Aaxonia qas ●nalyaln. A 40 mq nample h-aped on a
bubblt!d into the dried organic phasm square of ~andpap~r was plsced undmr
reqvnerated the •min~ and preclpltatml -n ●nvil and a 2.5 kq w~iqht was drop-
the d~slr.d smmonlum ualt, ADNT. Rm- @ cmto thr anvil. No tandpaixr In
crystatllsatinn in 90/10 Volum* ratlh urrrx! for typq !itl. An ]rbitrary l@v@i
●thyl ac@tate/acetone ●nd drying over

.*
 9. :!. Stincciphcr

Of SOUnd ● ‘90.9
indicattd The S08 ●ach pint (8). Energy of the e8pa5-
’90” hclght wan determined by the , slon waa compared to ~ by dlvidlng
Brucoton Up ●nd Down method [121.
ma thermal monaltivlty wes I
meawrod by tho ~ifiod IIonkln method:
●s dovoloped by Roqerm (13) ●nd I
JannQy. A thin slab o: ●xplomivo wan
comtlned in ● csrtridqo~ plac~d In ● I
tom~raturo Controlld bath of wood’s
•otal~ ●nd tlmod until ●mplomiorr. l%.
tomperaturo belo@ which it will not
●Epldo la tho critical temperature.

ThQ uedq9 to9t, a meaaurcof

dlatancc of run ● shock botoro
of det-
oimtlom starts in an ●xploslvQ, was
dome ●t Loa Ala-a by the Detonation
Physics qcoup fit) on 300-anq18
●ini-uodaos ■actlin~d Crom 2.54-cB-di4m
prcsaed ~LiI@ors. Theo. prwmur.a
war. uaad to find tho rolationahlp of
tho run to detonation, X*, to the
proamura input.

Performance Tests

Tlm deconatkon v~locity was

•mawr~d by two qroupm ●t bm Alamoa.
Tlm mthod us~d by the Detonation
Physics qroup has b~on dencribed by
8nqalkc (1S)1 it 1s very ●ccurate.
Tht Ias Ala-n Exploslven Technology
qroup’a mthai fOLIOuS.

Ionkzstlon mr~tchea ■ado o?

polymmirlo-insulated, four-m~l copper
wire wnro placed about 2.54 mm tpart
becuesn th- charqes. The pausaqe of
the tonkzod rletonaclun wavo Crkqqarrd
● t.lmor. ●ccurac~ to ● LO nano-
So:ondm . We umad a m~ack of SIS 2.54-
cm-diam charqm held tlqhcly Ln plac~
on ● 5.00-cm-thick •t~ol plat~ with
tap-. Tho dent was measur~d by ● ball
tnd rinq ●ethod. PlacQ danca of the
standard ●mplosivon hav? &en ~jr-
relatd by Ymlth [16) and Urlzar. For
this Z.S4--diam uncontln~d plata
dent teat, ● ftctnr of %.6U ❑ult~pliad
by t!l- dent f-) qw- th@ d~tenat~mt
premmrro fGPJlm

~llndor t~mta -r- done by Lhe

Los Alamo- Detonation Phymlcs yroup. ~
The sanpl~s wro fired Ln a 2.54-cm- I
lnnw-dlam by JO.4a-m-Lonq co-r i
tub- or ● 5.OU-cm-lnn@r diaa by
60.96---lcnq cnpper tu-. A atreah
camera recordd tho ●aparrJion of the
copp-r ●t ● milt 20.12 cm d-n th”
tub~ ●nd ●pproprimtcly scal~d In the
S.oa-ca tume. Th@ time Vmmua eapan-
●ion dtta were ●nalyzed by flttinq ●
pwcr curve thwuqh JO points bur-
roundlnq th~ 6-c 19-0 and JO-- Polnco
of ●xparmlcm ●nd b flndlnq th flrmt
dlftmcntlai for vcli=lty ●nd tho ■cc-
md dlffmmti~l fm ■ ccolcratiun ●t
 ?1. M. Stlneclpher

TABLE 1

sensitivity Tests

Haterial Impact Sensitivity Critical Temperature

@lar ratios) Type 12(cm) 12B(cm) Heakin (OC)

ADNT 58 225
ADNT 2H20 224 ---

AN ~320 361
1.38/l-AN/ADNT 66 236
2/1-AN/ADNT 65 241
2/l\l.3-AN/ADNT/TATB 2513 236
1.38/l/l.54-AN/ADNT/R.DX 37 215
5;l/1-AN/ADNT/RDX 44 219

5/1/l/3.3-AN/ADNT/RDx/Al 38 ~~1

EDD 88 245
2.33/l-AN/E!MJ 109 244
3.7/l/l-AN/Am4T/EDD 93 212
3/O.3/l.AN/ADN?/EDD 58 ~~7
FDEK 74 226
1.38/l/l.38-AN/ADNT/NQ 108 256
L.38/l/l.83-AN/ADNT/NQ 312 261
Y# ’320 198
RDx 22 214
TNT 15J 28.)

where:
AN ● ammonium nitrate
ADWT = mseonlum dinitrotr;azoiatc
EDD ● ethylenediamlnq (Ilnttrste
W = nitcWuafiidine
RDX ● cycLotrimrthyl@ne trinitramine
TATB ● 1, .1, 5-triaml*lo-2,4, b-trlnltcubenzene
TNT ● l, J,5-tr\nitrotoLuene
AL - aluminum

Shot
—.. ___ Shot
S*cond Thlrj
Firnt
—.— — . . .-. .—— - Shot
.. . .
;ensity (9/cm’) 1.640 1,640 1.640
Input PreR9Ute (CPa) 6.9 8.7 7,8
Run to D@tonatlon (m) 6.1 2s7 4.13
Time (~,e) 1.28 0.>5 0,30
 H. Y. Stincciphcr

sol

x WATf R

a~: I
b M
9 10 20 so
Omaln F(M}
w

FLq. L
Ralative Sh&k Scnsit Lvitien of 2/1
M4/ADWT and Other Explosives in the
Wt.dqe Teat.

%x 9s01 - 95/?.5/2.5 wtn M$lX/Est,lnc/-

!1P
PDX ~502 - 9S/$ wtt TAl13/Kcl-F 1100

bt@:, plate dent teats were CIOIU

in conjunction with rletonatlrm voloc~ty c
tcsta on 2.54-cm-dl~m charqes (Table 10
4). Ho found that the addition ot (cm)
● 8tra AN to t% wtectlc forrnulstlon
roducmd tho aqKocmont with the calcu-
Ldtal VI1lUCS With the elc@ptlm o;.th?! .“:1. .
aluminized 2/1 mnlar ratio ANYAIN4”:,
which porformd hettcr than calculated.
AIY”JI1
rL

(Flqure 21.

~ztr~pnl.tt~.l P.== ~~lc~l~td p:J

(~p~ ) (GPs
.--— .— — ~

l.?i-AwAwr 1,590 23.2 25.4

1.645 2).0 27.6

l,J#!l-AN/ADNT 1.6J0 27.J J6.7

1.%10 P’stld Z6.7

i.10/l/l.J@-AN/AUm/~ Imbst 26.1 20.0

l.)#11/l.’J-M/AD~/~X 1. 7oa J1.6 JO.4

i.3Q/L/i-M/AD~/M 1.?56 14.2 lJ.4

I
 3. A. Stineclphcr

TABLE 4

Unconflncd 2.54-cm Rate Stick/Plate Dent Tests

Haterlal I’xocrimencal CaiculaCed

(mlar ratlol Pr.y(dent)(GPn) D(-ls~ P-y(GPa) w

2/1-AN/ADNT 1.640 26.1 7U92~i 27.3 0268

l.Wl/l.S-AN/AD~/RDX 1.711 31.7 E455:2 30.6 8475
s/1/l-An/ADNT/sDx 1,699 24.0 771221 30.4 8598
5/1/l/3.3-AN/ADNT/RDx/Al 1.752 25.0 7739310 29.A 8223
2/1/2.66-AN/ADn/Al 1.734 26.3 7844 25.1 7680
2/1/l.3-AN/ADW/TATB 1.765 20.1 7a45:l :8.0 COIJ
L.3e/l/L.3e-AN/ADm/No 1.655 26.4 ------ :a.o a305
1.30/l/l.83-AN/ADNT/NO 1.654 25.5 dlbO :6.8 d197
J/L/l-AN/AM/CDD 1.607 24.2 ~b64~1 27.4 a207
3/o.3/L-AN/ADNT/EDD 1.535 20.ti .-.--- 93.0 7873

I.JI 1.10
1.13 1.4*
L.46 1.1)

i.no 1.1: ~.i~ 1,,18 1.1? 1,1” 1.:: :.?0 I.L$

1.09 1.11 !.:s 1.:4 L.9G 1.:1 1..G :ml~ 1.11
1.09 1.10 fL. baIb L.:1 L.00 I.L1 1.CI L.G6 1.10
 .

_rnw wcwnms~on ~m~-~ ● *-=--z ---- -- -. - .. —....—

Experimental Calculations ILL*L)

Denolty wam 1.639 qlcm]
121Jt12 1261:40 (from products]
-AH detonation (cal/g)

Products (ml/ml I!I?) BKWRCJ IsentroWl

15:OR lfj?su

1.7s. 1.77 1.70

H,0

1.47 1.49 1.49

!12

0.59 nm~”) ).59

CO*

~.:o)z 9.rJo2s
112 0.0096

,m::~l 1.0065
eo 0.0092

W Q.!2011 ~

w , 0.0006 !l.:.3U9 1.010

1).!)rlr)5 ~ )
IICY

v. 51scussIm

.
 !1. !!. Stinccipher

thero la ea. other factor, which 1s Another way to look at ideallty

hot obvioun now, that ■akes the dlf- 18 by ●eaauring the detonation prod-
Cerence. There ●re projects in pro- uctn and comparing the result with
qrema to find ways to decrease the what would be ●rpected for complete
particle ●ize of the AM in EDD;AN ■lz- reaction before freeze-out. The deto-
tures ●nd eearch for other explosives nation calorimetry ●xperiment (Table
that form ●utectlca with AN that wuld 6) ●hwed that the products from the
hsve different heats of formation. detonation of 2/1 molar ratio A!!/AD~,
the C02-balanced intermolecular for-
Another way to increase the ■ulation, were what was ●zpectd. The
tenperaturo in the detonation zone 1s oxyqen from the M ham been used by
to ●dd ●luminum ●ekal ~der. This the C or CO frm the ADNT to form
should help Increaso the ldeallty of C02 almost ●zcluslvely. The recov-
the performance because the tempera- ●ry of the products war ●zcelleltt be-
ture of the detonation affects the cause there were no aoiid prtiuccs.
layer thickness of a particle of M There is defln~tely complete reaction
that will react in the detonation zone in this case before Cre*z@-ouc at ●he
(19). We SOQ that this is the cane produc:s.
when qoinq frnm the mizcure 5/L/l
molar ratio AWADfwT/uX to one con- Aa we BCLMV these ●utecclc
talnlnq ●luminum, 5/1/l/l.J molar mystema dnd tind others, we kill bet-
ratio M/ADNT,’nDx/Al. The detonation ter understand the parsmeeers e=at ar-
sel~ity lncr~amed from 908 to 94* of Cect the renctlans between mol-ules
the calculated value. Addition of in the detonation zone.
●luminum to 2~1 molar ratio AN/ADNT
Increased D frnm 95Q to 102Q of th~ AcRwLE*;mEWS
calculated value. We testr~l the lat-
ter cc+omition In the 2.54-ea-dtam The authfir qr~at!y .~ppreelat~:l
cylinder test. W- found, .13 did the contrlb,l::onm Ia ?-can~ca: n-lp
P[nqer (20) and Bjarnholt (21), that ●nd underscand:nq qlven 3Y M,sr::m L.
●luminum b-hav-s ss an inert in the Clancy, ~. L. :lancy, C. E. Hsanatorl,
early part OF th~ ●xpanaion [6 m) but W. ?. rnz, Joan L. Janney, M. J.
keeps thm wall sccelerat~nq even at III Urtzar. ![. H. Cady, H. D. Ccburn, K:*1
me. The wall wloclty is almost aa Y, Lo~, a. P. Cnq@lk@, A. U. UsZPb@li.
Cant at 19 mm and is fsstmr than t!w c. w. !lautz, :. B. Raaley, .:. L.
projected value of ?hm 2?1 ~lar r.ltto Ma(ter, B. G. C:aLq, .lnd eapc:ally t:-
AN/ADWF St 10 ~ [Table 4). Th@ prn- support :Iy R. %. ltoq~r~ .tnd cJnver-
jected value was dotermln~d by .Iver- Sttlnna ● 1:5 :. Il. Akatm
●qinq the lncremantn @f thm nth~r cyL-
irrb: taatm thst h~ve D ●lwqt .lq cal- T5- wr~ wan support~d .= i~.trt
Culated. The tomts with D conal.lar- by th~ %SVI1l $ea 5yntens Command snd
obly Iea9 than Calculated showed a Naval Surf.ice Hmapons Center ::cxI
hiqher lncreano in wall v~loclty from proqras und~r ~~psrta~nt 01 fmr.ly
]9 t’a 10 m than thomm with D clrm? ta Contrsct w-74J5-ENG-M.
calculated.
REFEmcrs
W@ have dtacuosmd Ideall%’; .IS
Chc ahlllty of m intwrmnlmcular @E- 1. R. V. Rmt-cm, “4s Alama
ploalve to Coil- Calculated ~rfnrm- NstlOnfil :Atir.l!orv, As A1.t=jt.
ance as do th~ mn-lecullr ●xplo- N NM M*z;co, ~f:~:nal e-Mwli-
S1VQ9 that w~re uaaf tn calibrat= taq c,t~lmn, : 17?.
calcvlstlonom in th~ BW Calculatinnq
the mqroement is not too qood unless 2. M. Pinq@f. F. dmlm. E. “s, R.
tho ratios of tha ●lemmnta ■aklnq Up itost, P. lhwng, J. ws;ton, P.
the mu eaploaivo ●ro ●lmont the gSBQ Hay*m, and L. i’e~n, “tStr*ctrri -
●s in cho mudel compound, ROx. Many zation or Co-erc\al C-sit=
of th~ IntQrmol@cular @IplOBiVeO hsve Emploa\vQm,= pr=, g~m:~ Q~m-
● ■ uch hlqhar rstlrz of hydrwen to pcsium Ifntl) on >tonatlon~
carbnn than **s RDX ao they probably A@u@t 1?76, Cor,>nado,
would not tit
well.
● ta
~or ●mampl~,
the calculation ●s
tha RDX ha- C;H;O
rat10 1/2/2 mnd k.1U/1 AN/Adn
haa COli’O ● tom ratio lf4.7614.91 but
I Callfmrnia,
t=,trcll
7:9-)J9.
r-port
OffLca ~IC Naval
Adi.~21, ~.
RQ-

2.1)/1 wlar ratio AN/EDD han C;ll/o-. .

● to9 ratio l/’9.64.’4@4@.

4
 ?!. ‘!. Stinccipher

3. R. R. McGuire, D. L. Ornellaa, ; 11. R. Y. Lee, D. C. Ott, ard M. M.

●nd 1. B. Ak8t, ‘Detonation 9tineciphar. “Use of SoLvent Ex-
Chomlstryl Dlffuslom Control in’ traction in the Production ot
Non-Ideal Exploolvea,= Pro~l- the Ammonium Salt ot 3.5-
;;;;:,and Explosives, ~, 23 DinltroL,2,4-TriazoLe=, J. of

4. J.
.

IWmhkoultz, I. Akst, ‘A New

I
‘
Ind.

1901.
and Enq. Chain. Procemm DO-
sbqn and Dov., to be published,

~roach to Improvinq the Per-

formance of Non-Ideal EmploSivem 12. L. C. Smith and E. H. Eyeter,
Contalninq ~nium Nitrate,” ‘Phyelcal Testinq of Csploeives,
Plcatlnny Arsenal Technical Re- Part 111 - Miscellaneous Serial-
port 4789, March 197S. tivity Tests,= ~RD Report No.
5746, December 1945.
5. 1. Akat, J. WrahMmLtz, “lCspl*
■ iv. Performance Modiflcstlon by J3.
ComoLldLflcatLon of ~nium Nl-
trato with Puels,- PLcat~nny
Arsolal TechnLcal Report 4907,
October 1976. 14.

8. J. RermtikouLtx ●nd 1. Akat, “lm-

provamenc of Performance of Com-
posite ExpLomiv~s Containknq Am-
-n!um Nitrate by Phy~icaL Syn- L5.
thesis,= Proc. Sixth Sympslum
[Intl) on D@tOnatlOn, Auqumc
L976, Coronado, Cslifnrnta, 0[-
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7. n. S. RwlQr [now H. H.
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LA-7190-FUY, !ieptQmb*r 117am

0. 1. B. ‘~~tonation
Akrnt, in
IntQrmolmcular Explo~ivQs:
Characc@rlmtlca OC Some thrtmctke
?Ormul.ttlonm,” Prne. S*v-ntfr
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Juno L9al, Anna~Lio. !%ry:and.

9. L. 1. naqal, M. S. Pevfln@r, A.
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9ctrQludyakava, ‘Synt~*81s of
FJitro o~rlw~t~ws 01
,2,4-Triazoie. L,l,4-
T!timllaaq~-, y~trazol~, t,],4- 19.
Oxmdiaml-, ar,d Pyrazmle by th~
Noncacalytic fI@placwment nf tha
Diazo Group by the NitrO Grnup,-
Rhla. Get~ru. 9oe4., g, z5Q
[1970) .
da ●

10. L. 1. BwJ*l and M. 9. Pwzwr,

“Ac\d-Bsa@ PropQrti@m nf Nitro
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 Y. 3. Stincclphcr

21. G. Bjarnholt, ‘Effects of Alu- M. A. Cook, The Science of Hi h

minum and Llthlum Fluoride Ad-
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