DOD-P-16232P

7 November 197S
SUPERSEDING
MIL-P-16232E
15 OctQber 1974
(See Section 6)

MILITARY SPECIFICATION

PHOSPK4TE COATINGS, HEAW , MANGANESE OR

ZINC EASE (FOR FERROUS METALS)
I
‘L%is specification is approved fOr use by~~~ar.t=
;enta “and AgekcXes of the Department of Defense.

1. SCOPE

1.1 =. l%is specification covers two types of heavy phosphate

coating for ferrous metals, applied by iunneraion. The coatings consist
of a manganese phosphate or zinc phosphate base and, when specified, a
supplementary treatraent (see 6.1).

1.2 classification. Coatings shall be of the following types and

classes, as specified (see 6.2) :

● Type M Manganese phosphate base

class 1 Supplementary p reserv8 tive treatment or

coating, as specified

ClaB6 2 Supplementary treatment with lubricating oil

conforming to MIL-L-3150

Clasa 3 No supplementary treatment

Clase 4 Chemically converted (may be dyed to color as

specified) . W no supplementary coating or
supplementary coating as specified

Wnef icial comments (reconnnendations, additions, deletions) ,

and any pertinent data which may be of use in improving
this document should be addressed to:
Naval Ordnance Station, Standardization Division (611)
Indian Head, MU 20640, by using the self-addressed
Standardization Document Improvement Proposal (UO Form
~ 1426 a earin at the end of this document or h letter.

FSC-MFFF

I,1
DOD-P-16232F

Type Z 1 Zinc phosphate base

class 1 Supplementary preservative treatment or

coating, as specified

Class Z Supplementary treatment with preservative

conforming to MIL-C-16173, Grade 1 or
MIL-L-3150 (as alternate for very small parts)

class 3 No supplementary treatment

.
class 4 Chemically converted (gay be dyed to color
as specified) . With no wpplementary coating
or supplementary coating as specified .

z. AWLICASLE DOCIJNXNTS

2.1 Issues of documents. The followlng documents of the issue in

ef feet on date of invitation for bids or request for proposal, form a
part of this specification to the extent specified herein.

SPECIFICATIONS

FSDER&

TT-C-490 Cleaning Methods and Pretreatment of Ferrous

Surfaces for Organic Coatings

MILITARY

MIL-P-116 Preservation-Packaging, Methods of

MIL-L-3150 Lubricating Oil, Preservative, Medium

MIL-c-16173 Corrosion Preventive Compound, Solvent

Cutback, Cold-Application

MIL-P-50002 Phosphate Coating Compounds, For Phosphating

Ferrous Metal

* STANDASDS

MILITASY

MIL-STD-105 Sampling Procedure8 and Tables for Inspection

by Attributes

MIL-STD-121g ACS Chemicals

2
DOD-P-16232F

(Copies of specifications, standards, drawings, and publications

required by contract~rs in connection with specific procurement
functions shodd be obtained from the procuring activity or as directed
by the contracting of ficer.)

2.2 Other publications. The following documents form a part of this

specification to the extent specified herein. Unless otherwise
indicated, the issue in effect on date of invitation for bids or request
for proposal shall apply.

AMERICAN PUBLIC HBALTH ASSOCIATION AND AMERICAN WATERWORKS ASSOCIATION

Standard Methods for the Examination of Water and Waste Water,

13th Edition, 1971

(Applications for copies should be addressed to tbe American Public

Health Association, 1015 lBth Street, NW, Washington, DC 20036, or the
American Waterworks Association, 2 Park Avenue, New York, NY 10016).

AMERICAN SOCIETY FOR TESTING AITONATERIALS (ASTM)

ASTM E 8 Tension Testing of Metallic Materials

ASTM B 117 Salt Spray (Fog) Testing

10 (Applications for copies should be addressed to tbe American Society

for Testing and Materials, 1916 Race Street, Philadelphia, PA 19103) .

Af.iSRICANNATIONAL STANDARDS INSTITUTE (NSI )

B46.1 - 1962 Surface Texture

(Applications for copies should be addressed to tbe American

National Standards Institute, Inc. , 1430 Broadvay, New York, NY 10018).

(Technical society and technical association specifications and

standards are generally available for reference from libraries. They
are also distributed among technical groups and using Federal agencies. )

3. R5QUIRElCiNTS

* 3.1 Preproduction inspection. Unless otherwise specified (see 6.2) ,

a preproduction inspection is required and shall be used to verify
that the process complies with 3.2. Details of the procedure, chemicals,
and the equipment proposed to be used by the contractor shall be sub-
mitted in writing via the contracting officer to the procuring activity,

!0
DOD-P-16232F

and written approval shall be received from the contracting officer

prior to production.. The exact designation of all materials proposed
for use, together with the names of the manufacturers, shall be stated.
The proposed procedure shall include a detailed method of control, with
limits for time, temperature, pH values, and all other pertinent details
that will ensure compliance with the requirements of this specification.
No deviation from the approved process shall be permitted without prior
written approval of the procuring activity. Approval of process, ntater-
ials and equipment implies no guarantee of acceptance of the results
obtained in use. Regardless of the processes or materials approved, the
phosphate coatings shall conform to all the applicable req”iremente of
this specification.

3.2 Process. The phosphate coatings shall be applied mder the

controls and in the stages described below. A single contractor shall
perform all phases of the coating process. Unless otherwise specified
(see 6.2) , phosphate coatings shall be applied after all machining,
forming, t..eldi”g,and stresa relieving heat treatment have been completed,
but prior to hydrogen embrittlement relief treatment.

3.2.1 Bath materials and controls. The bath materials and controls
of the bath shall be In accordance with the following:

* a. The materials used in the baths ehall be capable of producing

phosphate coatings conforming to all requirements herein for the type and
class specified. Government activities shall use materials In accordance
with MIL-P-50002 (see 6 .4.1).

b. The bath concentration, temperature, and immersion time for

parts shall be euch that the phosphate coating meets all the requirements
of this specification.

c. The equipment shall be constructed of materials resistant

to the action of the phosphating solutions and free from copper alloy
fittings or brazing in contact with the solution.

d. Phosphatized parts shall not be allowed to dry between the

phosphatizing solution treatment and the subsequent cold ruining water
rinse. Fog sprays or other mee.ne for prevention of drying shall be provided.

* e. The supplier of the phosphate coated parts shall maintain a

permanent record (gee 3.2.lg) of the history of each processing bath,
showing all additions of chemicals to the bath, and the resulte of all
analyses performed.

f. Control of the chemical content of the phosphate coating

baths shall consist of determination of free acid, total acid, and ferrous

4
DOD-P-16232P

iron. Unless otherwise specified (see 6.2) , the frequency of testing for
chemical content shall be determined by the user but must be sufficiently
frequent to assure adequate control so that it can be demonstrated that
no lot of parts is processed when the bath is not within the established
limits. AI’Ialysisfor free and total acid should be made just prior to
the processing of each lot or every two houre, whichever is less frequent.
The ferrous iron content should be analyzed just prior to the processing
of each lot or weekly, whichever is less frequent.

g. Permanent records of bath controls shall be maintained for

not less than one year (seven when specified csee 6.2)) and made available
to the Government upon request. Permanent records shall be defined as
legible reco’rdsflrinted tn ink”or tvped in lieu of pencil led notes.

● 3.2.2 Stage 1, cleanin~. Cleaning shall be in accordance with

i- method 1, II, III, or 2V of TT-C-490, or a combination thereof under
the follovi.ng conditions. Abrasive blasting is the preferred treatment
prior to heavy phosphating and shall be utilized unless otherwise
specified and/or approved by the procuring activity (see 6.2) for
reasons of dimensional control or surface finish roughness control that
make it neceesary to omit abrasive blasting (Bee 3.2.2.l.d and 6.5) .

3.2.2.1 Rust or scale remova’1. Rust or scale shall first be

removed by dry, abrasive blasting using sand or steel grit 10 accordance
with method I of 2T-C-490 under the following c.mditions:

● a. Parts shall be free of oil, grease, dirt, and other contamination

or else degreased before abrasive blasting.

b. Abrasive tumbling shall not be used.

c. After blasting, any abrasive residue shall be removed by a blast

of dry, compressed air.

* d. Abrasive blasting shall be controlled and performed using a grit

size sufficiently fi~e t“opreserve the required RMS surface finish
roughness. mere abrasive blasting will damage the finish, method
III, V or VI of TT-C-490”may be used to remove light rust provided they
do not adversely affect tbe coating quality. Strong acids or alkaline
solutions shall not be used prior to manganese base phosphate coating
without subsequent surface conditioning to refine the coating grain and
reumve the effects of such solutions on the surface reactivity and the
phosphate coating process Csee 6.5) .

3.2.2.2 ~. kT_ten
m-?thod 111 or IV of
TT-C-490 is used, cleaning shall be folloved by a thorough rinsing in
clean vater.

5
DOD-P- 16232F

I 3.2.3 ~ hosphatin . The phosphate coating shall be applied

by immersion under the following conditions:

~ * ~. Type M coatings shall be manganese base and type Z shall be zinc

base. All materials used for coatings shall be approved by the procur-
Ing activity as Specified in 3.1 or shall be in accordance with KIL-P-50002.
1 .,
b. The bath concentrations, temperature, and immersion time for
parts shall be such that the phosphate coating meets all the require-
ments of this specification.

* 3.2.4 Stage 3, water rinde. The clear cold water rinse shall be
performed in accordance with the following:

a. Dip rinsing: A continuous oveT flow shall be maintained by the

addition of fresh water. Items shall be Iwnersed only as long as Is
necessary to meet the requirements of this specification.

b. The flow of rinse water shall be adjusted, regulated or

controlled (e.g. by conductivity controllers) in conjunction with the
rate of production in order to prevent its contamination at any time
I
beyond a limit that is such as to assure no detrimental effect on the
I coatings produced.

c. Spray rinsing may be utilized provided the same end product

●
quality is maintained.

1 d. Immediately following the water rinse, all items (except

class 4) shall be treated in the chromic acid rinse of stage 4 (see 3.2.5) ,

3.2.5 Stage 4, chromic acid rime (classes 1, 2 and 3) . The chromic

acid rinse of classes 1, 2 and 3 shall be performed in accordance with
I the following:

*’ a. The final rinse shall be hot 65 to 939C (150 to 200”F) chromic

acid or chromic-phosphoric acid”solution: approximately 300 grams
chromic acid flake in 1000 liters (L) water.

b. The final rinse shall be maintained at a PH of 2 to 4 by the

addition of flake chromic acid Or mixtures Of chr~ic and phOsphOric
acids.

I* c. The final rinse shall be checked by a standard free and total

acid titration or PH reading as often as is necessary to assure that

I the bath remains within the limits set at all times during which it
is in operation.

I * ‘“ All rinses should be discarded whenever they become ccmtami”ated.

The final rinse shall be checked at least weekly a“d shall be discarded
when the total acid reading rises to more than 7 times the free acid reading.
I
6

—
DOD-P-1 6232P

e. The item should remain in each rinse for a mlnlmum of 60 Second(B) .

f. Following the chromic acid rinse, the item shall be tlioroughly

dried before application of a supplementary treatment, as applicable.

● 3.3 Stress Relief. Unless othervise apecif ied (see 6.2) , parts
(including carburized parts) having the minimwn hardness value of 39
Rockwell C and which are ground, cold formed or cold straightened shall
be given a streaa relief heat treatment 177 to 204°C (350 to 400”F)
for a minimum of one hour(h) for every inch of thickness but not less
than half hour before cleaning and coating.
* 3.4 Hydrogen embrittlement relief heat treatment.

1- 3.4.1 Unless otherwise specified (see 6.2) , parts (including carbur-

ized parts) having the hardness values shown In TASLE I shall be given
a hvdroEen embrlttlement relief heat treatment after coatinz uer TABLE I
wit~out-any parts developing cracks.
1 3.4.2 Unless othervise specified (gee 6.2) , all lots of parts or
material for which baking is required and subject to a sustained load
In service exceeding 25 percent of the base metal yield strength shall
be tested for hydrogen embrittlement.
I ● TAELE 1. Hydrogen embrittlement heat treatment.

●
I

I Stage of operation

Heat treatment for

I both types of coat-
ings and material
is conducted after
coating but before
any stressing
I operation

7
DOO-P-16232F

* 3.5 Weight of phosphate coatinRs. The weight of phosphate coacings,

prior to application of any supplementary treatment, shall conform to
the following:

a. Type M shall be a minimum of 16 grams per square meter (g/mz)

(11 g/m2 when specified (see 6.2))

b. Type Z shall be a minimum of 11 g/m2

3.6 Accelerated corrosion resistance. The phosphate coated item,

free of supplementary treatment, shall be subjected to a salt spray
(fog) test. It shall show no evidence of corrosion for the period of
time shown in TASLE II. When authorized by the procuring activity
(see 6 .2), the Springfield immersion test may be used in lieu of the
salt spray test.

3.7 Supplementary treatments. Supplementary treatments shall be

applied after completion of the phosphating procese in accordance with
the followim. Items receivin!z mmolementarv
.. treatment shall be either
centrifuged or permitted to drain sufficiently to remove all surplus
from tbe surfaces.

3.7.1 Types M and Z, class 1. The supplementary treatment for

class 1 of types M and Z shall be as specified (see 6.2) . Unless
otherwise specified, weight of oil per unit area does not apply.

TASLS II. Accelerated corrosion resistance requirement

(free of supplementary coating) .

coat ~ system Sxposure time, minimum

I
Type class Salt spray, h Springfield immersion
test, minutes
I
M 1 1-1/2 I 10
M 2 1-1/2 10
M 3 1-1/2 10
M 4 24

z 1 2 10
z 2 2 10
z 3 2 10
z 4 24

s
DOD-P-16232F

I 3. 7.2 Type M, Ch313 2. The supplementary treatment for class 2 of

type M shall be impresmation with lubricating oil conforming to mL-L-3150
(equivalent to P-7 of MIL-P-116) . Unless otherwise specified (see 6.2) ,
the weight of oil per unit area shall be such that items show m signs
of corrosion when subjected to the salt spray test for a minimum of 24 bores.

3.7.3 Type M, class 4 ~ystems. Type II, class 4 systems shall be

manganese base phosphate coatings that have been chemically converted by
I reaction with a reagent containing an inorganic salt. When specified
I (see 6.2) , items shall receive supplementary treatment or be dyed to a
specific color after chemically converting the phosphate coating. class
1. 4 coatings shall show no signs of corrosion when subjected to the salt
spray test for a minimum of 72 hours only if supplementary treatment
is applied.

3.7.4 Type Z, class 2. Type Z. class 2 coatings shall be impreg-

1“ nated with corrosion preventative conforming to grade 1 of MIL-C-16173.
I When specified (see 6 .2), as an alternate method, it shall be permissible
to impregnate very small parts with lubricating oil co”f.orming to
I MIL-L-3150. Unless otherwise approved ceee 6.2) , the weight per unit
area of corrosion preventative shall be euch that items shall show no
aigna of corrosion when subjected to the salt spray test for a minimum
of 48 hours.

3. 7.5 Type Z, claBs 4 systems. Type Z, class 4 systems shall be

zinc base phosphate coatings which have been chemically converted by
reaction with a reagent containing an inorganic salt. When specified
(see 6.2) , items shall receive supplementary treatment or be dyed to
a Epecific color after chemically converting the phosphate coating.
Class 4 coatings shall show no sigrm of corrosion when subjected to the
salt spray test for a minimum of 72 hours only if supplementary treat-
ment is applied.

3.S Dimensions of coated items. Items shall comply with dimensional

requirements of the drawinga prior to application of the phosphate coating.
After coating, Items shall comply with the dimensional requirements of
the drawings, with allowance for the phosphate coating buildup. (For
interference in close fits, see 6.6).

3.9 Surface texture. Items shall comply with the finish or surface
texture requirements of the drawings prior to application of the phosphate
coating and after coating when the coating has been stripped as described
in 4.8.4.1. Surfaces for which the required characteristics can only be
obtained by special mechanical or elect ro-mechanical OPeratiOns shall
be so specified for proper phosphating. Surface texture, as specified,
shall be interpreted in accordance with ANSI B46. 1.

I
I 9
I

DOD-P-16232P .(, :

3.10 Workmanship. Phosphate coatings shall .be evenly deposited, and

shall have a uniform crystalline
. texture with a Dattem not readilv
visible to the unaided eye and shall not produce any evidence of etching
or intergranular attack of the base metal. Coatinga shall be grey to
black, and shall not have a mottled appearance. They shall be free of
white stains (due to dried phosphating solution) ,,rust, and ‘fingerprints.
However, brown or orange s tsins caused by chromic acid rinse and non-
uniformity of color due to heat treatment, degree of cold wprk, or
composition of the base metal shall not be cause for rejection.

4. QUALITY ASSURANCE PROVISIONS

4.1 Responsibility for inspection. Unless otherwise specified in

the contract, the contractor is responsible for the performance of all
inspection requirements as specified herein. Except as otherwise specified
in the contract, the contractor may use his own or any other facilities
suitable for the performance of the inspection requirements specified
herein, unlese disapproved by the Coventment. The Government reserves
the right to perform any of the inspections set forth In the specifi-
cation where such inspections are deemed necessary to assure that
supplies and services conform to the prescribed requirements.

* 4.2 Classification of inspection. The Inspection requirements

specified herein are classified as follows:

a. Preproduction inspection csee 4.5)

b. Quality conformance inspection (see 4.6) ●
* 4.3 Inspection condf tions. Unless otherwise specified (see 6.2) ,
all inspections shall be performed under the following conditions :“

a. Temperature: SDOm ambient 18 to 35°C. (65 to 95”F)

b. Altitude: Normal ground
c. Vibration: None
d. Humidity: Room ambient to 95 percent relative, maximum.

● 4.4 Sampling.

4;4.1 Preproduction sample. When specified by the procuring activity

(see 6.2), preproduction samples of the item or items co be phosphate
coated in accordance with the contract or other similar items approved
by the procuring activity shall be coated using the methods and procedures
apprOved in accordance with 3.1. The number of samples shall be as
specified in the contract (see 6.2). The sample items shall be subjected
to the preproduction inspection detailed in 4.5 at an activity designated
by the procuring activity (see 6.2). Acceptance of the preproduction

10

I
I
DOD-P-16232P 1-=-

sample shall’be based on no defects in the sample. Furth&’ production by

I the contractor prior to approval of the preproductfon sa@le shall be.
,,
I at the.contractor’.s risk.

I * 4.4.2 Lot size. Unless otherwise specified (6ee 6J2),’a lot shall “-.”.’
consist o-ated items of the saue base metal composition, type and “
I clasa of coating, trea~ed under the same c.mditions, during’one shiftj ‘%. “
in the same processing baths of approximately the same size ‘~d shape, “
and to be submitted fo< acceptance at one time. In addition,,where
I continuous or conveyor equipment is used, a lot shall CCM.ISiStof ~
1. maximum of four conaec”tive hours of production.

* 4.4.3 Quality conformance inspection samplin&.

...” .1.
1.
4.4.3.1 samp ling for examination. Unless othervise specified (sic’6.2),
I a random mmple of coated items shall be taken from each’’lot in accordance
with inspection level II of MIL-STO-1O5, and subjected ~o the quality ‘“
I
conformance examination as specified in 4.6.
I ,-
4.4.3.2 SamPling for tests. Unless otherwise specified (see 6“.2),
I
s~ltng for teStB shall be in accordance with the following:

a. Process control terms. Sampling for process control testing

shall be ,as established by the contractor and approved by the procuring
activity. The sampling plan shall be sufficient to demonstrate adequate

‘o control of the proceea and confomr.ante of products processed to the require-

ments of this specification.

b. Quality conformance teats. A random sample of coated items

shall be taken from each lot in accordance with inspection level S-1 of
UIL-STD-105 and subjected to the quality conformance tests as specified
in 4.6.

c. Stress and hydrogen embrittlement relief test. Unless “

othervise specified (see 6.2), testing for determination of the adequacy
of treatment for the relief of hvdrogen embrfttlement shall be performed
by the processor at a frequ6ncy ;sta~liihed by him which shal~be
demonstrated to assure freedom from failure caused by hydrogen embrittle-
ment by his process for each”bath or process line and each type of .’.’.
material processed. ...
,,=..
* 4.5 Reproduction Inspection. The preproduction inspection shall *
consist of obtaining approval as specified in 3.1 of procedure, che.mical~~
and equipment proposed to be used by the contractor for production and,,
”
when specified (see 6.2), the tests and examinations specified in TASLS 111
performed on sam+les selected in accordance with 4.4.1.

11

p
--- - . . . . . .
uuu-r-m~xt

● 4.6 Quality conformance inspection. The quality conformance

inspection shall consist of the tests and examinations specified in
TASLE 111 uerformed on samples selected in accordance with 4.4.3. The
stress and hydrogen embrit~lement test shall be performed for each lot
only when specified by the procuring activity (see 6.2) . Records of
bath controls and history shall be maintained by the contractor and
made available to the Government upon request as specified In 3.2.1 e
and g.

4.7 Examinations.

● 4.7.1 Process examination. The contractor shall allow examination

of the phosphate coating procees, upon xequest from the procuring
activity, to verify conformance with 3.2.

☛ 4.7.2 Coated item examination. Samples selected in accordance with

4.4.3.1 shall be examined for compliance with the requirements of
3.g, 3.9 and 3.10. Dimensional and surface roughness measurements
after application of the coating need be made only when specified by
the procuring activity (bee 6.2). The acceptable quality level (AQL)
shall be 1.5 percent defective.

4.8 ~. The AQL for quality conformance tests shall be 4.0

percent defective.

4.8.1 Test specimens. Teat specimens shall be in accordance

with the”following:
e
a. If the sfze, shape or cost of the coated item is such that
\tests cannot reasonably be performed on the item, separate representative
t>st suecimens ma.?be utilized. These test specimens shall be supplied
by the contractor-. Such test specimens shall be cut from scrap items
or tide from the same alloy, heat treated in the same manner, and Surface
finished by the same process as the items they represent. The specimens
shall have an external surface area of frmn 10 to 100 square centimeters
(cmz) except aB noted in 4.8.3.

b. The test specimens shall be distributed randomly and processed

concurrently with the items.

c. The test specimens shall be used only once and then discarded.

● 4.8.2 Process control tests. Process control teats shall be performed

at the frequency established in accordance with 4.4. 3.2.a. to verify
conformance with 3.2.1 through 3.2.5. The contractor’s standard procedures
shall be used as approved per 3.1.

12
TABLE 111. Preproduction and quality conformance inspection .

Preproduction Quality conformance

Test or examination Requirement Method inspection inspection

Bath materials and controls 3.2.1 4.7.1 and 4.B.2 X x

Cleaning 3.2.2 4.7.1 and 4.8.2 x x
Phosphating 3.2.3 4.7.1 and 4.B.2 x x
Water rinse 3.2.4 4.7.1 and 4.8.2 x x
Chromic acid rinse 3.2.5 4.7.1 and 4.8.2 x x
Stress and hydrogen
embrictlement relief 3.3 and 3.4 4.8.3 x (See note 1)
Weight of coating 3.5 4.8.4 x x
Accelerated corroeion 3.6 4.8.6 x x
Supplementary treatment 3.7 4.8.5 x x
Dimensfona of coated items 3.8 4.7.2 x x
Surface texture 3.9 4.7.2 x x
Workummhip 3.10 4.7.2 x x

Notes: 1. The atrese and hydrogen embrittlement test shall be performed on each lot only when specified
by the procuring activity (see 6.2).
DOD-P-16232P

4.8.3 Stress and hydrogen embrittlement relief. Testing for relief

of stress and hydrbgen errbrittlement shall be performed in accordance with
the follovf.wg:

a. Samples of parts that will be subjected to a sustained tensile

load in use (see 6.2) shall be subjected to a sustained tensile load
equal to 75 percent of tbe tensile yield strength of the material.

* b. Unless otherwiee specified (see 6.2), the parts shall be held

under the load for at least 200 hours and then examined visually under
10x magnification and an illumination of 1100 lux(lx) for cracks. The
lot shall be rejected if any coated part develops any crack.

c. Parts which require special fixtures or extreme loads to

comply with the above requirements shall be tested as specified by the
procuring activity Csee 6.2).

* d. For eteals having mininmm tensile strength of 1655 megapascals

(MPa) or hisher, cylindrical specimens in accordance vith Figure 8 of
ASTM E8 with a 0.51 nm notch in the center of the gage length shall be
used for teat. The area at the base of the notch shall be one-half that
of the full diameter of. the spectien. The notch shall have an angle
of 60”. The radius at the base of the notch shall be 0.254 ? ?.013 nun
for standard 12.8 WM diameter specimens and proportional to this for smaller
specimene. These parts shall be subjected to a sustained teneile load
equal to 75 percent of the ultimate notch tensile strength of the material.

4.8.4 Weight per wnit area of phosphate coatings.

4.8.4.1 ‘@e M coatings. Weight per unit area of phosphate

coatings prior to supplementary treatint shall be determined in
accordance with the follovi.ng:

a. Weigh the coated ,teat epecimen to the nearest fag; remove

the coatings by Inmersi&n for a minimum of 15 minutes in a 50 gram per
liter (g/L) chromic acid stripptig solution at approximately 74°c (165”F);
rinse in clean, running water; dry and reweigh.

b. Repeat the procedure until a constant weight is obtained.

The chromic acid solution @hall not be reused.

● c. If a supplementary treatment is present, it shall be removed

prior to testing by immeraicm in a solvent such as petroleum ether or
1,1,1-trichloroethane. The coating weight shall be calculated as
follows :

14
DOD-P-16232F ... ~

d. Calculation: Weight per unit area of phosphate coating,

w (glmp)= (Initial weight in grams-final weight in grams)

Total area in square meters

4.8.4.2 Type Z coatin~. Weight per unit area of type Z coatings,

prior to supplementary treatment, shall be determined in accordance with
the following:

a. Weigh the coated test specimen to the nearest mg; remove the
coatings by imrersfon at room temperature for a minimum of 10 minutes In
a stripping solut%on conforming to TABLS IV. (If desired, the chromic
acid stripping solution described in 4.8.4.la may be used. )

b. Rinse in clean, running water, dry, and reweigh.

c. Repeat the procedure until a constant weight is obtained.

●
d. If a supplementary treatment is present, it shall be removed
I prior to testing as described in 4.8.4 .lc. The coating weight shall be
calculated as described in 4.8.4 .ld.
I
I TA8LE IV. Stripping solution for type Z coatings.

4.8.5 Weight of supplementary treatment. Weight per unit area of

suppl~ntary treatment shall be determined in accordance with the
follm..ing:

a. Age the test samples fOr a minimum of 16 hours at room temperature,

or dry at approximately 51.5°C [125”F) for a minimum of 3 hOurs. cool
I in a desiccator and weigh accurately.
I
b. Completely remove the supplementary treatment by immersing
I in successive baths of petroleum ether or naphtha, or by l,l,l-trichloro-
I ethane vapor decreasing.

c. Rinse the sample in alcohol, dry, and reweigh.

15
DOD-P-l6232F

d. Determine the weight of the treatment per unit area “sing

the following calculation:

e. Calculation: Weight per unit area of supplementary treatment,

W(g/m2) - (Initial “eight in grams-final weight in granm~

area in square meters

4.8,6 Accelerated corrosion resistance. Accelerated corrosion

resistance shall be determined in accordance with 4.8.6.1 or 4.8.6.2
under the conditions specified for each test.

4.8.6.1 Salt spray (fog). Accelerated corrosion resistance by

salt spray (fog) shall be performed in accordance with the following:

a. Subject the samplee co a 5 percent salt spray tee.

t as
described in AS’IM B 117.

b. Exposure times for coatings tested prior to supplementary

treat~nt shall be in conformance with TABLE II.

c. Exposure time of coacings tested after application of supple-

mentary treatment shall be in accordance with 3.7.

4.8.6.2 Springfield immersion test. If authorized by the procuring

activity (see 6.2), the Springfield irmnersion test may be used in lieu of
the salt spray test for teacing phosphate-coated articles prior to
application of a supplementary treatment. The test shall be performed
in accordance with the following:

a. Apparatus and conditions: Appar.tus,capable of providing the

proper control of aeration, temperature, velocity, and pH of the sol”ticm
shall be used to insure adequate reproducibility. See FIGUSE 1 for a
schematic diagram of typica3 apparatus suitable for this test.

b. Tmk : The tank shall be constructed of nmterIal =eBiatmt to

attack by aerated salt water at elevated temperatures. Glass, fibrous
glass-reinforced plastic, or rubber is considered satisfactory for this
purpose. The tank shall be of sufficient size to provide at least
1.OL of solution for each 19b cmz of specimen surface, and there shall
be sufficient additional volume to allow a thermostat sensing element,
stirrer, pH meter electrodes, and heating elements to be immersed in
the bath. The tank may be rectangular vlth internally rounded corners
(see FIGUSS 1), and should be fitted with a lid to facilitate temp.zra-
ture control and to exclude dust and other contwninants.

16
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DOD-P-16232F

r- THER”os,A,

II

- FIGuRS 1. Schematic dtagram of Springfield

Immersion Teat Apparatus.

c. Aeration, air regulation, and purification: The bath shall

be aerated with a regulated flow of air which has heen freed of carbon
dioxide. The stretuoof air used to aerate the bath shall be regulated
hy passage through a pressure regulator and a calibrated flowmeter at
the rate of 50 cm3 per minute per liter of test solution. The regulated
stream shall be freed of carbon dioxide by pasaage through a tower
packed with a solid absorbent for C02, such as “Ascarite” or soda-lime.
The COZ absorbing tower shall be connected in the air line between the
pressure regulator andzthe flowmeter Csee FI~ 1). A tower 6.4 cm in
diameter and 24 cm in height has been found satisfactory for this purpose;
for high rates of air flov, it may be necessary to employ tvo or amre
towers connecced in parallel. If “Ascarite” is used, the tower shall
be recharged with fresh “Ascarite” when the color of the absorbent has
changed from vhite to grey.

17 I

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DOD-P-16232F

● ’
d. Air saturation: To obtaim air maturation of the test solution,
the regdated and purified stream of air shall be blown through a gas
dispersion tube having e 20 mm diameter, coarse- fritted glass disk on
tbe end, to break the air stream .into small bubbles. Saturation of
the bath usually requires approximately one hour. The solution shall
be saturated with the air prior to the test, and aeration shall be
continued during the test. The degree of saturation may be determined
by the Winkler test for dissolved oxygen (see American Public Health
Association and American Water Works Association, Standard Methods for
the Sxaminatlon of Water and Waste Water, 13th Edition, 1971).

e. Temperature control: The temperature of the bath shall be

maintained at 65 f 2°C (149 i 3“F) during the test by use of a bimetallic
therroo-regulator in conjunction with one or more 500-watt immersion
heaters sheathed in fused silica, quartz, glass, or other material
resistant to attack by the bath solution.

f. Solution velocity: A fluid velocity of 0.2 m/s e.hallbe

maintained in the solution during the test by means of an impeller type
pump or a variable-speed zig-zag stirrer. The fluid velocity may be
determined by measuring the time required for a float on the surface
of the bath to travel a definite distance.

g. pH control: The pH of the solution shall be maintained between

6.8 and 7.0 during the test. The pH may be measured by means of a pH
meter having an immersion-type electrode assembly. Dilute sodium
hydroxide or hydrochloric acid may be added to the solution as required
to maintain the PH within the specified llmits.

h. Specimen supports: The supports for the test specimens shall

insulate the specimens from each other and shall allow free contact
of the specimens with the test solution. . The supports shall be made
of a material which will not be attacked by the corroding solution.
Glass, Plastic lRmfnate B and varnished wood have been found to be
satisfactory materials for use in supporting specimens.

4.8.6 .2.1 Test solution. The test solution shall be in accordance

with the following:

Preparation: The test solution shall be prepared accurately

usin~”sodium chloride conforming to MIL-STD-1218. The solution shall
contain 2.0 percent by weight of sodium chloride in freshly boiled
distilled water stored in a container made of glass, polyethylene, or
other material that will not contaminate water. The cmenlnz of the
container shall be connected to towers packed with “Ascarit=” or soda-
lime to protect the water from atmospheric C02.

18

1
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DOD-P-16232F :,

I b. Volume: There shall be at Leaet 1.0 L of solutlon fob each

194 cmz of specimen surface area to minimize changea in corrosivenbsa
of the solution or accumulation of corrosion products i“ .tbe bath. The
I solution shall be discarded after it has been used to test specimens “
having a combined surface area of 194 Cmz per liter or after a one-day
I run if a smaller area hae been tested. The volume of the test solution
shall be maintained constant by the addition of boiled distilled water
to offset any increase in salt concentration.
I
I 4.8.6 .2.2 Tent specimens. The test specimms shall be in accordance .
with the folloving:
1.
a. Number of specimens: The number of specimens tested at one .
I
time in a bath shall be limited by the ratio of the surface area of
1. specimen to the volume of test solution (see 4.8.6 .2.la).
I b. Preparation of specimens: Samples shall be subjected to
I vapor-phase decreasing with 1,1,1-trichloroethane to free them of oil
or grease, rinsed in alcohol, and force-dried at approximately 60°C (140”F).

c. Test procedure: After being immersed in the bath for a

minimum of ten minutes under conditions specified in 4.8.6.2, the specimens
shall be examined to determine compliance with the requirements of 3,6.

5. PACKAGING

‘a * 5.1 ~ ackagin acking and markin . Preservation,

packaging, packing and marking for shipment of phosphate coated parte
.:..

shall be in accordance with the applicable parts specification.

6. NOTES

6.1 Intended use. The phosphate coatings covered by this specifi- ..

cation are intended for use where “heavy” coatings are required. Light .
phosphate coatings used as a paint base are covered by other specifi-
cations, such as TT-C-490. However, “heavy” phosphate coatings may
be used as a paint base where required on some Naval Gun Systems and
Assemblies.

6.1.1 -. Type M coatings are more resistant than Type z to

alkaline environments. Type M coatings shodd not be exposed to
temperature in excess of 121°c (250”F). Except for special purpose
applications, phosphate coatings should be used with a suitable supple-
mentary treatment. Each class for type M is described below:

a. Class 1 EI11OVS the procuring activity to specify a suitable

supplementary treatment depending upon the particular application.

I 19
DOD-P-16232P

b. Class 2 covers coatings impregnated with MIL-L-3150 lubr-

icatingoil. l%la class may be specified for general purpoee applications
in which a moderate degree of corrosion resistance is required and to
prevent wear and assist in the “breaking-in” of bearing surfaces.
MIL-L-3150 oil may be removed from phosphate coated items by contact
with absorbing material.

c. Class 3 covers coatlnfzswithout surmlmnentarv

.. treatment. This
class is intended for special purposes in vhicb a supplementary treat-
ment is not desired.

d. Class 4 covers chemically converted coatings, chemically

converted with supplementary treatments that are suitable for use where
corrosion protection is required in addition to other properties (see 1.2).
l%fs coating is recommended for use where a dyed or colored coating such
as olive drab or a black (non-reflective) coating is needed. The class
4 coating provides improved corroeion resistance; however, the supple-
mentary coating provides most of the corrosion protection vhen used in
conjunction vith DhOsDhate coatinR8. The class 4 coating provides an
f.mp%ved “break-i& c&ting and ii recommended for red.c~n~ the sliding
I friction in preference to the class 2. The use of the class 4.coating
reduces the variation in torque versus tension values usually found
with threaded fasteners.

6.1.2 Type Z . Type Z coatinge should not be used if contact’with

alkaline materials or exposure to temperatures above 93°C (21)O”F)is
expected. Type Z coatings may be used to prevent galling in cold-
extrusicm and deep-drawing applications. Except for special-purpose
●
applications, Type Z coatings should be used with a suitable supple-
mentary treatment (see 1.2).. Each class for type Z is described below:

a. Clas8 1 allowa the procuring activity to specify a suitable

treatment depending upon the particular application.

b. Class 2 covers coatings impregnated with grade lof MIL-C-16173.

lhis slaBB may be specified for general purpose application in vhich
corrosion vrotectfon is the primary consideration and where a “dry-to
touch” film is required, indoor or outdoor, for domestic and overseas
shipment, with or without cover. MIL-c-16173, grade 1 compound is
I equivalent to P-10 fl:.
MIL-P-116.

c. Class 3 covers coatings without supplementary treatment.

~ie class is intended for special purposes IIIwhich a supplementary
treatment is not desired.

20

●
DOD-P-L6232F

●
d. Class 4 covers chemically converted coatings vith ~upplem.entary
treatments that are suitable for use where petroleum base or wax supple-
mentary treatmence cannot be used but where extended corrosion protection
is necessary. The color of tbe chemically converted coatings will be
grey (see 1.2). Class 4 chemically converted coatings, treated with
a high melting wax or a preservative oil, provide excellent corrosion
protection where the wax or oil is not objectionable. 3%is coating is
recommended for use where a dyed or colored coacing such as olive drab
or a black (non-reflective) coating is needed. The class h coating
provides improved corrosion resistance; however, the supplementary coating
provides most of the corrosion protection when used in conjunction with
phosphate coatings. The clasB & coating provides an improved “break-in”
coating and is recommended for reducing the sliding friction in preference
to the class 2. The use of the clasB f+coating reduces the variation in
torque versus tension values usually found with threaded fasteners.

6.2 Ordering data. Procurement documents should specify the

following:

* 6.2.1 Procurement requirements.

a. Title, number and date of this specification.

I b. TYPe and class of coating (see 1.2).

c. hhen preproduction inspection is not required csee 3.1 and 6.3).

d. When phosphate coating (and any supplementary treatment) is

not to be the final process (see 3.2).

e. When frequency of bath sampling is not the contractor’s option

(see 3.2.1P).
t
f. Wlen abrasive/blasting is not required as pretreatment (see 3.2.2).

When stress and hydrogen embrittlement relief is not required

(seeg~.3 and 3.4).

h. h%en type M coating weight shall be 11 g/m2 (see 3.5).

I
i. When Springfield immersion test is allowed (see 3.6 and 4.8.6.2).

j. Supplementary treatment required for class 1 and weight of

treatment (pee 3.7.1).

k. When weight of e.upplemencary treatment for class 2 is ocher

than as specified (see 3.7.2 and 3.7.4).

21
DOD-P-16232F

1. Supplementary treatment and color of dye desired for type M

or type Z, class 4 (see 3.7.3 and 3.7.5) , when applicable.

m. Inspection conditions if other than as specified (see 4.3).

n. Assigned activity for preproduction inspection (see 4.~.1).

o. Number and type of preproduction samples required.

D. Specify if any excepticm to lot size and sampling plans

(8ee”4.4.2 and 4.4.3.1).

q. When stress and hydrogen embrittleu,ent relief tests are

required for each lot; frequency if not for each lot; exceptions and details
of procedure (see 4.4.3.2c, 4.6, TAsLE III and 4.8.3).

r. When tests and examinations are required for preprod”cticm

inspection (see 4.5).

s. When surface roughness and dimensional measurements are

required after coating (.nee4.7.2).

* 6.2.2 Contract data req”lreme”ts. Any data required for delivery

in connection with this document shall be specified o“ a DD Form 1423
incorpo~ated into the contract. Such data will be delivered as identified

● ’
on completed (numbered) DIDs (Data Item Dee.criptions/DD 1664) which will
be documented in the Applicable ADL (Authorized Data List).

● 6.3 Preproductlon sample waiver. Prepreoduction samples submitted

and approved on a recent contract may be accepted by the procuring activity
in lieu of an additional preproduction sample inspection. Wlen the
preproduction sample is waived (see 6.2.lc), the procurement document
should contain a statement specifying that the standards of workmanship
exhibited by the previously approved preprodwtion sample shall determim
the rninumnn requirement~ of the current contract or order.

6.4 Supersession data. ‘CABLEV shows the classification comparison

of this specification with coatings specified in previous editions of
NIL-P-16232 and MIL-c-12968.

6.4.1 Phosphating materials. Phosphating solutions previously

includedlin MIL-P-16232 are now covered in MIL-P-50002. Phosphating
materials complying with MIL-P-5DO02 should be procured and used by
Government agencies to produce coatings conforming to MIL-P-16232.

* 6.5 Surface finishes finer than 0.80 ❑icrometers. Abrasive blasting

using too coarse a media grit size may destroy surface finishes less

22
DOO-P-16232F

than 0.80 micrometers. The grit size must be Belected to be compatible

with the surface finish requirement and it may b? necessary to use 320
Eric size or grade 1000 class beads. Phmmhate coatiras should not be u.

specified for highly polished surfaces that cannot tolerate fine vapor
abrasive blasting. Phosphate coating is not recommended for surfacea
of ,0.20micrometers or less (see 3.2.2.ld).

TAfU V. Classification comparison.

DoD-P-16232F
& MIL-P-16232E MIL-P-16232D MIL-P-16232C kIL-p-16232B !L-C-16Z32A WIL-C-1Z968

Type M,Class 1 ~pe M,Class 1 Tm M,WSS 1 TYP$.M,CISSE : ~e A

!-
Type M,Class 2 rype M,Class 2 TYPE M,ClaBs Z Type M,Class : Type I
Type M,Class 3 Type M,Class 3 Type M,Class 3 Type M,class :
t- Type M,Class 4 rype M,Clasa 4& Type M,Class 4
New Class 4 rype M,class 41 Type M,Class I+B - —
deleted
4A,B,C,6 D

rype M,Class 4C F’ -
rype M,Class 4D -
rype M,Class 4E -
1
Type Z,Class 1 rype Z,Class 1 Type Z,Class 1 Type Z,class 1 Ype B,Class 1
Type Z,Class 2] rype Z,clatm 2] Type Z,ClasB 22 Type Z,class 2 Type II

● Type Z,Class
Type Z,Class
3
4
ryee Z,Class
rype Z,Class
3
4A
Type
Type
Z,Class
Z,Class
3 <Type Z,Class
4A Type Z,Class
3
4 we B,ClaBs 2
New Class 4 rype Z,Class 4B Type Z,Class 4B -
deleted rype Z,Class 4C Type Z,Class hC -
4A,B,C, 6 D Type Z,Class 40 Type Z,Class 4D -
l’ypeZ,Class 4E Type Z,Class 4E -

1 Treated”witb MIL-C-16173, Grade 1 (or MIL-L-3150 for very small parts).

2 Treated with MIL-C-16173, Grade 2.
I 3 Treated with MIL-c-16173, Grade IA.

~ ‘:~~ VI gives expected thickness

6.6 Dimensions of coated items’.
I of phosphate coatings. If close fits are apecifi=d, buildup in thick-
ness caused by the phosphate coaciag may result in apparent interference
I o“ assembly. Coatings are friable, hovwer, and assembly may be
accoiaplishedby forced fitting, wiping, or othemtise removing the
I surplus coating. Nonferrous metal wire brushes should not be employed.
I Salt spray or Immersion test requirements are applicable to coated
articles prtor to removal of any coat’ingin assembly operations.

23
DOD-P-16232F

TABLE VI. Sxpected tNc!iness of phosphate coatinga.

● 6.7 Changes from previous issue. The margins of this specification

are marked with an asterisk to indicate where changes (additions,
modifications, corrections, deletions) from the previous issue were
.pade. This vas done as a convenience only and the Government assumes
no liability t?hataoever for any inaccuracies in.these notations.
Bidders and contractors are cautioned to evaluate the requirements of
this document based on the entire content irrespective of the marginal
notations and relationship to the last previous ise”e.

Custodian : Preparing Activity:

ARMY-m NAVY - OS
NAVY - 0s Project Number:
A2R FORCE - 11 MPPP-0128

Review Activities:
ARMY -MI, AV, EL
●
NAVY - AS, SH

.—

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24

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