ASTM D800-91(1997)
(Test Method)Standard Test Methods of Chemical Analysis of Industrial Metal Cleaning Compositions
Standard Test Methods of Chemical Analysis of Industrial Metal Cleaning Compositions
SCOPE
1.1 These test methods describe the procedures for the chemical analysis of industrial metal cleaning compositions in solid, paste, or liquid form. These cleaning compositions may contain caustic alkalies, silicates, phosphates, chromates, carbonates, bicarbonates, borates, sulfates, sulfites, nitrates, chlorides, soaps, rosin, sulfonated wetting agents, anti-foaming agents, organic bases, organic solvents, organic coupling agents, and sometimes inorganic acid salts or organic acids. Occasionally, such cleaning compositions may contain sulfonated oils; in such cases, reference should be made to Method D500. The examination under a low power microscope or magnifying glass, supplemented by a few qualitative tests, will often indicate the number of components and their identity.
1.2 The analytical methods appear in the following order: Section Preparation of Sample 4 Total Alkalinity as Na2O 5 to 7 Total Fatty Acids (and Rosin) 8 and 9 Na2O Na[inf]2[r]O 5 to 7 Total Fatty Acids (and Rosin) 8 and 9 Na[inf]2[r]O Combined with Fatty Acids (and Rosin) 10 and 11 Anhydrous Soap 12 Rosin (McNicoll Test Method): Qualitative 13 and 14 Quantitative 15 to 18 Total Silica Calculated as SiO[inf]2[r] 19 to 22 Phosphates: Qualitative 23 and 24 Quantitative 25 to 32 Combined Sodium and Potassium Oxides 33 to 36 Chlorides 37 to 39 Sulfates 40 to 42 Water Distillation Test Method 43 to 46 Carbon Dioxide by Evolution-Absorption Test Method 47 to 51 Loss at 105[deg]C 52 and 53 Total Matter Insoluble in Alcohol 54 to 56 Free Alkali 57 to 59 Synthetic Detergent or Wetting Agent 60 and 61 Volatile Hydrocarbons 62 to 66 Loss on Ignition 67 and 68 Report 69 and 70
1.3 This standard does not purport to address all of the safety problems, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.> Material Safety Data Sheets are available for reagents and materials. Review them for hazards prior to usage.
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Designation:D800–91(Reapproved 1997)
Standard Test Methods of
Chemical Analysis of Industrial Metal Cleaning
Compositions
This standard is issued under the fixed designation D 800; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (e) indicates an editorial change since the last revision or reapproval.
This standard has been approved for use by agencies of the Department of Defense.
1. Scope
Free Alkali 57-59
Synthetic Detergent or Wetting Agent 60 and 61
1.1 These test methods describe the procedures for the
Volatile Hydrocarbons 62-66
chemical analysis of industrial metal cleaning compositions in
Loss on Ignition 67 and 68
Report 69 and 70
solid, paste, or liquid form. These cleaning compositions may
contain caustic alkalies, silicates, phosphates, chromates, car-
1.3 This standard does not purport to address all of the
bonates, bicarbonates, borates, sulfates, sulfites, nitrates, chlo-
safety concerns, if any, associated with its use. It is the
rides, soaps, rosin, sulfonated wetting agents, anti-foaming
responsibility of the user of this standard to establish appro-
agents, organic bases, organic solvents, organic coupling
priate safety and health practices and determine the applica-
agents, and sometimes inorganic acid salts or organic acids.
bility of regulatory limitations prior to use. Material Safety
Occasionally, such cleaning compositions may contain sul-
Data Sheets are available for reagents and materials. Review
fonated oils; in such cases, reference should be made to
them for hazards prior to usage.
Method D 500. The examination under a low power micro-
2. Referenced Documents
scope or magnifying glass, supplemented by a few qualitative
tests, will often indicate the number of components and their
2.1 ASTM Standards:
identity.
D 500 Test Methods of Chemical Analysis of Sulfonated
1.2 The analytical methods appear in the following order:
and Sulfated Oils
Section D 841 Specification for Nitration Grade Toluene
D 843 Specification for Nitration Grade Xylene
Preparation of Sample 4
D 1193 Specification for Reagent Water
Total Alkalinity as NaO5-7
Total Fatty Acids (and Rosin) 8 and 9
Na O Combined with Fatty Acids (and Rosin) 10 and 11
3. Purity of Reagents and Materials
Anhydrous Soap 12
3.1 Purity of Reagents—Reagent grade chemicals shall be
—Rosin (McNicoll Test Method):
Qualitative 13 and 14 used in all tests. Unless otherwise indicated, it is intended that
Quantitative 15-18
all reagents shall conform to the specifications of the Commit-
Total Silica Calculated as SiO 19-22
tee onAnalytical Reagents of theAmerican Chemical Society,
Phosphates:
Qualitative 23 and 24
where such specifications are available. Other grades may be
Quantitative 25-17
used, provided it is first ascertained that the reagent is of
Combined Sodium and Potassium Oxides 33-36
sufficiently high purity to permit its use without lessening the
Chlorides 37-39
Sulfates 40-42 accuracy of the determination.
Water, Distillation Test Method 43-46
Carbon Dioxide by Evolution-Absorption Test Method 47-51
Loss at 105°C 52 and 53
Annual Book of ASTM Standards, Vol 15.04.
Total Matter Insoluble in Alcohol 54-56
Annual Book of ASTM Standards, Vol 06.04.
Annual Book of ASTM Standards, Vol 11.01.
Reagent Chemicals, American Chemical Society Specifications, American
These test methods are under the jurisdiction of ASTM Committee D-12 on Chemical Society, Washington, DC. For suggestions on the testing of reagents not
Soaps and Other Detergents and are the direct responsibility of Subcommittee listed by the American Chemical Society, see Analar Standards for Laboratory
D12.12 on Analysis of Soaps and Synthetic Detergents. Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
Current edition approved July 15, 1991. Published September 1991. Originally and National Formulary, U.S. Pharmaceutical Convention, Inc. (USPC), Rockville,
published as D 800 – 44. Last previous edition D 800 – 89. MD.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D800–91 (1997)
3.2 Unless otherwise indicated, references to water shall be TOTALFATTYACIDS (AND ROSINACIDS)
understood to mean reagent water conforming to Specification
8. Procedure
D 1193.
8.1 Pour into a separatory funnel the neutral ethyl ether-
4. Preparation of Sample water mixture obtained from the titration in Section 6, using
additional ether to wash all the fat or oil into the separatory
4.1 Samples of metal cleaning compositions shall be well
funnel.Allowthetwolayerstoseparate,anddrawoffthewater
mixed. Excessive exposure to the air shall be avoided to
layer into a second separatory funnel. Wash the water layer
prevent the sample from absorbing moisture and carbon
with two 10-mL portions of ethyl ether. Combine the ether
dioxide and, if a volatile solvent is present, to prevent
extracts, and wash with successive portions of water until they
evaporation.
are no longer acid to methyl orange. Transfer the ether layer to
4.2 Solid Cleaners—If the cleaner is a solid and appears to
a weighed flask, evaporate the ether over a steam bath, and
contain no volatile solvent, dissolve 10.000 g in freshly boiled
finally dry to constant weight at 105°C.
water and dilute to 500 mL as the sample for analysis.
4.3 Liquid or Paste Cleaners—If the cleaner is a paste or
9. Calculation
liquid dissolve a sufficient portion in freshly boiled water to
9.1 Calculate the percentage of fatty acids (and rosin acids)
give the equivalent of 10.000 g of the dry material in solution,
as follows:
and dilute to 500 mL as the sample for analysis.
Total fatty acids ~and rosin acids!,% 5 ~E/W! 3 100 (2)
NOTE 1—In order to prepare this sample it is first necessary to
where:
determine the water content (Sections 43-46), loss at 105°C (52 and 53),
E = grams of ether residue, and
and volatile hydrocarbons (Sections 62-66).
W = grams of sample used.
TOTALALKALINITYAS NA O
NA O COMBINED WITH FATTYACIDS
(AND ROSINACIDS)
5. Reagents
5.1 Ethyl Ether.
10. Procedure
5.2 HydrochloricAcid, Standard (0.5 N)—Prepare and stan-
10.1 Dissolve the fatty acid (and rosin acid) residue ob-
dardize 0.5 N hydrochloric acid (HCl).
tained under Section 8 in warm neutral alcohol, add six drops
5.3 Methyl Orange Indicator Solution
of phenolphthalein indicator solution, and titrate with 0.5 N
NaOH solution.
5.4 Sodium Hydroxide, Standard Solution (0.5 N)—Prepare
and standardize a 0.5 N sodium hydroxide (NaOH) solution.
11. Calculation
6. Procedure 11.1 Calculate the percentage of Na O combined with the
fatty acids (and rosin acids) as follows:
6.1 Pipet 50 mL of the sample (1.000 g) prepared in
Na O combined with fatty acids ~and rosin acids!,%
accordance with Section 4, into a 250-mL Erlenmeyer flask.
Addmethylorangeindicatorsolutionandameasuredexcessof
5 ~B 3 0.0155!/W 3 100 (3)
0.5 N HCl, and boil to expel carbon dioxide (CO ). Cool, add
25 mL of ethyl ether, and titrate the excess HCl with 0.5 N
where:
NaOH solution. When the water layer is neutral to methyl
B = millilitres of 0.5 N NaOH solution (1 mL of 0.5 N
orange, it should be clear unless sodium metasilicate (or other
NaOH = 0.0155 g of Na O), and
silicate) is present in large quantities. If silicates are present,
W = grams of sample used.
they will form a gelatinous mass which will produce a
troublesome emulsion. All the soap will have been decom- ANHYDROUS SOAP
posed during the reaction and the corresponding fatty acid will
12. Calculation
be found in the ether layer.
12.1 Calculate the percentage of anhydrous soap as follows:
7. Calculation
H 5 C 3 0.29 (4)
7.1 Calculate the total alkalinity as percentage of sodium F 5 R 2 H
oxide (Na O) as follows:
2 P 5 F 1 C
Total alkalinity as Na O,% 5 A 2 B 3 0.0155 3 100 /W (1)
@~ ! #
where:
C = percentage of Na O combined with fatty acids (and
where: rosin acids) (Section 10),
A = millilitres of 0.5 N HCl (1 mL of 0.5 N HCl = 0.0155 F = percentage of fatty acid anhydride,
H = percentage of water equivalent,
gofNa O),
B = millilitres of 0.5 N NaOH solution, and R = percentage of fatty acids (and rosin acids) (Section 9),
W = grams of sample used. and
D800–91 (1997)
Complete this acidification and washing in a very short period
P = percentage of anhydrous soap.
of time, and keep the beaker covered to prevent oxidation of
ROSIN (McNICOLL TEST METHOD) theacids.Afterthelastwashing,removethelasttracesofwater
Qualitative
from the beaker with a pipet, filter the fatty acids through one
or two thicknesses of filter paper, and dry at a temperature of
13. Reagents
105°C for 45 to 60 min or heat rapidly to 130°C and allow to
13.1 Acetic Anhydride (99 to 100 %). cool. Do not hold at 130°C, but if water is present, decant the
13.2 Sulfuric Acid (34.7 + 35.7)—Prepare by carefully add-
clear fatty acids into another beaker, and again reheat them
ing 34.7 mL of H SO (sp gr 1.84) to 35.7 mL of water. momentarily to 130°C. These acids may then be used for the
2 4
rosin determination.
14. Procedure
17.2 Esterification and Titration—Weigh about 2 6 0.001 g
14.1 The presence of rosin may be determined qualitatively of the fatty acids into the esterification flask. Add 25 mL of
by testing a portion of the residue obtained under Section 8 by
naphthalene-b-sulfonic acid solution.Add a few glass beads to
the Liebermann-Storch reaction as follows: ensure smooth boiling, attach the reflux condenser, and boil for
14.1.1 Dissolve a portion of the ether extract by warming in
30min;also,runablanktestusing25mLofthereagent.Atthe
several times its weight of acetic anhydride, and then cool the
end of the boiling period cool the contents of the flask, add 0.5
solution.Allow several drops of H SO to flow slowly into the
mL of phenolphthalein indicator, and titrate immediately with
2 4
acetic anhydride-fat mixture. Rosin is indicated by the devel-
0.2 N alcoholic KOH solution.
opment of a fugitive violet coloration changing to a brownish
tinge at the margin of contact of the reagents. The test should
18. Calculation
becheckedbytestingasampleoffattyacidstowhichrosinhas
18.1 Calculate the results as follows:
been added. If the test for rosin is positive the quantitative
R 5 S 2 B! 3 N3 0.346 3 100 /W (5)
@~ #
procedureshouldbecarriedoutasdescribedinSections15-18.
R 5 R 2 1.0
Quantitative
R 5 ~R 3 F!/100
2 1
R 5 R 3 1.064
15. Apparatus
S 2
15.1 The apparatus shall consist of a glass flask connected,
where:
preferably by a ground-glass joint, to a reflux condenser.
R = percentage of rosin acids in fatty acids,
15.1.1 Esterification Flask—A 150-mL flask of either the
R = corrected percentage of rosin acids in fatty acids
round-bottom or Erlenmeyer type shall be used.
(Note 2),
15.1.2 Reflux Condenser—Any suitable water-cooled, glass R = percentage of rosin on basis of original sample,
reflux condenser may be used. R = percentage of rosin soda soap on basis of original
S
sample,
16. Reagents
S = millilitres of KOH solution required for titration of
the sample,
16.1 Naphthalene-b-Sulfonic Acid Solution—Dissolve 40 g
B = millilitres of KOH solution required for titration of
of Eastman grade or equivalent reagent in 1 L of absolute
the blank,
methyl alcohol.
N = normality of the KOH solution,
16.2 Phenolphthalein Indicator Solution (5 g/L)—Dissolve
W = grams of sample used,
0.5 g of phenolphthalein in 50 mLof neutral redistilled alcohol
F = percentage of total fatty acids (and rosin acids) in the
and then mix with 50 mL of water.
cleaner, and
16.3 Potassium Hydroxide Solution (0.2 N)—Accurately
A = percentage of total anhydrous soap (Section 12).
standardize a 0.2 N solution of potassium hydroxide (KOH) in
18.2 If true fatty acid soap is desired, subtract the rosin soap
neutral redistilled alcohol (due to volatility of alcohol, this
from the total anhydrous soap.
solution should be restandardized frequently).
16.4 Sulfuric Acid (1 + 2)—Carefully mix 1 volume of
NOTE 2—Cooperative studies have shown that the McNicoll test
concentrated sulfuric acid (H SO , sp gr 1.84) into 2 volumes method gives results approximately 1 % higher than the amount of rosin
2 4
present. Consequently, the committee recommends deducting 1 % from
of water.
the percentage of rosin found in the fatty acids.
17. Procedure
TOTALSILICACALCULATEDAS SiO
17.1 Preparation of Fatty and Rosin Acids—Dissolve a
sufficient portion of the sample to give the equivalent of 50 g
19. Reagents
of dry material in 500 mL of hot water. (If the cleaner to be
19.1 Hydrochloric Acid (sp gr 1.19)—Concentrated hydro-
tested contains alcohol, the alcohol should be completely
chloric acid (HCl).
removed by evaporation from the solution.) Add 100 mL of
19.2 HydrochloricAcid(1 + 1)—MixequalvolumesofHCl
H SO (1 + 2), and heat gently until the fatty matter collects in
a clear layer. Siphon off the aqueous acid layer, add 300 mLof (sp gr 1.19) and water.
hot water, boil gently for a few minutes, and siphon off the 19.3 Hydrofluoric Acid (sp gr 1.15)—Prepare a solution of
aqueous acid layer. Wash the acids in this manner three times. hydrofluoric acid (HF) having a specific gravity of 1.15.
D800–91 (1997)
19.4 Sulfuric Acid (sp gr 1.84)—Concentrated sulfuric acid
A = grams of ignited residue before treatment with HF
(CH SO ).
2 4 (21.3),
B = grams of ignited residue after treatment with HF
20. Preparation of Sample
(21.4), and
C = grams of sample used.
20.1 When Soap is Present—If soap is present in the
cleaner, draw off the water solution from the total alkalinity
PHOSPHATES
titration (Section 6) into a porcelain evaporating dish. Add an
Qualitative
excess of HCl (sp gr 1.19), evaporate the mixture to dryness on
a steam bath, and carry out the procedure in Section 21
23. Reagents
. The weight of the sample will be 1.000 g.
20.2 WhenSoapisNotPresent—Ifsoapisnotpresentinthe 23.1 Nitric Acid (1 + 5)—Mix 1 volume of concentrated
nitric acid (HNO , sp gr 1.42) with 5 volumes of water.
cleaner, transfer a 100-mL aliquot of the sample solution
obtained as described in Section 3 to a 400-mL evaporating 23.2 Silver Nitrate Solution (85 g/L)—Dissolve 85 g of
silver nitrate (AgNO ) in water and dilute to 1 L.
dish, neutralize with HCl (sp gr 1.19) using methyl orange as
the indicator, evaporate to apparent dryness on a steam bath, 23.3 Sodium Hydroxide Solution (1 + 1)—Dissolve sodium
hydroxide (NaOH) in an equal weight of water. When using,
and carry out the procedure as described in Section 21. The
weight of the sample will be 2.000 g. decan
...
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