MIL --- D TL --- 211F
4.2.3 Inspection procedure.
4.2.3.1 For examination of packaging. The sa mple unit sha ll be one fille d shipping conta ine r
re a dy for shipme nt. Sa mple shipping conta ine rs sha ll be e xa mine d for the following de fe cts:
Conte nts pe r conta ine r not a s spe cifie d
(a)
Conta ine r not a s spe cifie d
(b)
Conta ine r closure not a s spe cifie d
(c)
Conta ine r da ma ge d or le a king
(d)
Ma rking incorre ct, missing, or ille gible
(e)
Ba g e xte rior or drum inte rior or e xte rior conta mina te d with re d phosphorus
(f)
4.2.3.2 For test (see 6.6). Approximately equal portions of all of the specimens taken in 4.2.2.2
shall be thoroughly mixed to form a composite specimen of no less than 450 g. The composite speci-
men shall be tested as specified in the applicable portions of 4.2.4. Each test shall be conducted in
duplicate analysis. Failure of either analysis of any test shall be cause for rejection of the lot repre-
sented.
4.2.4 Tests (see 6.6)
(a) Inductive Coupled Plasma (ICP). Be sure a ll gla sswa re is fre e of me ta ls. Soa k gla ss-
wa re in 5% H NO 3, rinse with distille d wa te r, soa k in 5% H Cl a nd rinse with distille d wa te r.
Run ICP a ccording to ma nufa cture rs spe cifica tion. Assure the ICP ha s be e n purge d with nitro -
ge n a t 223.008 nm for Cu, 238.204 nm for Fe , a nd 177.494 nm for P. Ca libra te the instrume nt
using sta nda rds of Cu, Fe , a nd P. Run a wa te r bla nk be fore running sa mple s.
(b) Chemicals. Wa te r, in a ccorda nce with ASTM D 1193, a nd re a ge nt gra de che mica ls
sha ll be use d throughout the te sts. Whe re a pplica ble , bla nk de te rmina tions a nd sta nda rds sha ll
be run a nd corre ctions a pplie d whe re significa nt. ICP sta nda rds for coppe r a nd iron sha ll be 5
m /ml a nd sta nda rds for phosphorus sha ll be 50 m /ml. Te sts sha ll be conducte d a s follows:
g
g
4.2.4.1 White Phosphorus. Weigh 10 g of the RP specimen and add 50 milliliters (ml) carbon
disulfide. Mix for 60 minutes in a sonic bath or with magnetic stirrer. Filter through a Whatman No.
42 filter paper or equal and take a 10 ml aliquot into a 50 ml volumetric flask and allow to evaporate
dry in hood with air or nitrogen stream. Add 25 ml water, 2.5 ml concentrated nitric acid and dilute
to volume with water. Run ICP on prepared solution.
Pe rce nt White Phosphorus = 25 x 10 ---3A
W
whe re :
A=
ICP re a ding (m /ml)
g
W=
we ight of spe cime n (g)
4.2.4.2 Acidity as Phosphoric Acid. We igh 10 g of the R P spe cime n in a 50 ml fla sk a nd dilute
to volume with wa te r. Mix in sonic ba th for 5 minute s. F ilte r through a Wha tma n No. 42 filte r
pa pe r or e qua l a nd run ICP on solution.
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