Designation: D 126 – 87 (Reapproved 2002)

Standard Test Methods for

Analysis of Yellow, Orange, and Green Pigments Containing
Lead Chromate and Chromium Oxide Green1
This standard is issued under the fixed designation D 126; 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 2. Referenced Documents

1.1 These test methods cover procedures for the chemical 2.1 ASTM Standards:
analysis of yellow, orange, and green pigments containing lead D 280 Test Methods for Hygroscopic Moisture (and Other
chromate and chromium oxide green. Matter Volatile Under the Test Conditions) in Pigments2
1.2 The analytical procedures appear in the following order: D 521 Test Methods for Chemical Analysis of Zinc Dust
Sections (Metallic Zinc Powder)2
CHROME YELLOW, CHROME ORANGE, AND MOLYBDATE ORANGE D 1013 Test Method for Determining Total Nitrogen in
Organic Colors and Lakes 7
Moisture and Other Volatile Matter 8
Resins and Plastics2
Matter Soluble in Water 9 D 1193 Specification for Reagent Water3
Lead Chromate 10 and 11 E 11 Specification for Wire Cloth Sieves for Testing Pur-
Total Lead 12
Sulfate 13 and 14
poses4
Carbon Dioxide 15
Molybdenum 16 and 17 3. Summary of Test Methods
Extenders 18-22
Calculation of Substances Other than Insoluble Lead
3.1 Chrome Yellow, Chrome Orange, and Molybdate Or-
Compounds 23 and 24 ange:
PURE CHROME GREEN AND REDUCED CHROME GREEN 3.1.1 Organic colors and lakes are determined qualitatively
Organic Colors and Lakes 25
Moisture and Other Volatile Matter 26
by boiling the sample in water, then ethyl alcohol, and finally
Matter Soluble in Water 27 chloroform.
Iron Blue 28 3.1.2 Moisture and other volatile matter are determined in
Lead Chromate 29 and 30
Barium Sulfate and Insoluble Siliceous Material 31 accordance with Test Method A of Test Methods D 280.
Total Lead 32 3.1.3 Matter soluble in water is determined by boiling in
Sulfate 33 water and filtering.
Calcium Oxide Soluble in Acid 34 and 35
Extenders 36 3.1.4 Lead chromate is determined by dissolving the sample
Calculation of Insoluble Lead Com- in dilute HCl, filtering and titrating potentiometrically with
pounds 37 FeSO4 solution after addition of HClO4.
CHROMIUM OXIDE GREEN
Organic Colors and Lakes 38 3.1.5 Total lead is determined by precipitation as lead
Moisture and Other Volatile Matter 39 sulfide solution with H2SO4 and final precipitation as lead
Matter Soluble in Water 40 sulfate.
Total Chromium as Chromium Oxide 41
3.1.6 Sulfate is determined by dissolving the sample in
1.3 This standard does not purport to address all of the acetic acid, neutralizing with sodium carbonate, plus addition
safety problems, if any, associated with its use. It is the of HCl to an aliquot followed by addition of BaCl2 to
responsibility of the user of this standard to establish appro- precipitate as barium sulfate.
priate safety and health practices and determine the applica- 3.1.7 Carbon dioxide is determined by evolution.
bility of regulatory limitations prior to use. Specific hazard 3.1.8 Molybdenum is determined by precipitation as the
statements are given in Note 3. sulfide, solution in HNO3 and H2SO4, addition of NH4OH and
H2SO4. The solution is reduced in a Jones reductor, collected
under Fe2(SO4)3 solution and titrated with KMnO4 solution.
1
3.1.9 Extenders are either:
These test methods are under the jurisdiction of ASTM Committee D01 on
Paint and Related Coatings, Materials, and Applications and are the direct
responsibility of Subcommittee D01.31 on Pigment Specifications. 2
Annual Book of ASTM Standards, Vol 06.03.
Current edition approved May 29, 1987. Published July 1987. Originally 3
Annual Book of ASTM Standards, Vol 11.01.
published as D 126 – 22. Last previous edition D 126 – 65 (1981)e1. 4
Annual Book of ASTM Standards, Vol 14.02.

Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.

1
 D 126
3.1.9.1 Calcium carbonate, calcium sulfate, magnesium car- Society, where such specifications are available.5 Other grades
bonate or; may be used, provided it is first ascertained that the reagent is
(a) (a) The compounds in 3.1.9.1 are determined qualita- of sufficiently high purity to permit its use without lessening
tively by precipitation with ammonium solution. the accuracy of the determination.
(b) (b) If chromium is present, it is reduced and the lead 5.2 Water—Unless otherwise indicated, references to water
salts dissolved in dissolving solution. Hydroxides and hydrous for use in the preparation of reagents and in analytical
oxides are precipitated by addition of HCl and NH4OH and procedures shall be understood to mean reagent water con-
filtered. CaC2O4 is precipitated with calcium oxalate solution forming to Type II of Specification D 1193.
and filtered, ashed and weighed as CaO. Alternatively, the 6. Preparation of Sample
precipitate is dissolved in H2SO4 and titrated with KMnO4.
6.1 Mix the sample thoroughly and take a representative
Magnesium is determined on the filtrate from calcium deter-
portion for analysis. Reduce any lumps or coarse particles to a
mination by precipitation as the phosphate with ammonium
fine powder by grinding. Grind extracted pigments to pass a
phosphate solution.
No. 80 (180-µm) sieve (Note 1). Discard any skins that do not
3.2 Chromium Oxide Green: pass through the sieve. Thoroughly mix the finely ground
3.2.1 Organic colors and lakes are determined qualitatively pigment and preserve in stoppered and suitably identified
by boiling the sample in water, then ethyl alcohol, and finally bottles or containers.
choloroform.
NOTE 1—Detailed requirements for this sieve are given in Specification
3.2.2 Moisture and other volatile matter are determined in E 11.
accordance with Test Method A of Test Methods D 280.
3.2.3 Matter soluble in water is determined by boiling in 6.2 Moisten the weighed portions of extracted pigments
water and filtering. with a small amount of suitable wetting agent (Note 1) before
adding reagents for analysis.
3.2.4 Total chromium as chromium oxide is determined by
dissolving the sample in dilute HCl, filtering and titrating NOTE 2—A 0.1 % solution of sodium dioctylsuccinosulfonate has been
potentiometrically with FeSO4 solution after addition of found satisfactory. (This material is sold under the trade name of Aerosol
OT.) Wetting agents containing mineral salts, sulfates, or sulfonates which
HClO4.
may be hydrolyzed to sulfates, should be avoided; the use of alcohol is
also undesirable because of its tendency to reduce chromates.
4. Significance and Use NOTE 3—Warning: As the National Institute for Occupational Safety
and Health has stated that hexavalent chromium compounds are hazardous
4.1 These test methods are for analysis designed as an aid in
to health, care should be exercised in preparation of the sample. The
quality of yellow, orange, and green pigments containing lead wearing of a respirator and rubber or synthetic gloves are recommended.
chromate and chromium oxide green. Some sections may be If hexavalent chromium materials come in contact with the skin, wash
applicable to analysis of these pigments when extracted from thoroughly with soap and water.
whole paints.
5
Reagent Chemicals, American Chemical Society, Specifications, American
5. Purity of Reagents and Water Chemical Society, Washington, DC. For suggestions on the testing of reagents not
listed by the American Chemical Society, see Analar Standards for Laboratory
5.1 Reagents—Unless otherwise indicated, it is intended
Chemicals, BDH, Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
that all reagents shall conform to the specifications of the and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
Committee on Analytical Reagents of the American Chemical MD.

CHROME YELLOW, CHROME ORANGE, AND MOLYBDATE ORANGE

(Primrose, Lemon, and Medium Yellows; Chrome Oranges; Lead Molybdate or Basic Lead Chromate; Molybdate Orange)

ORGANIC COLORS AND LAKES tested for by reference to procedures given in standard refer-
ence works.6
7. Procedure MOISTURE AND OTHER VOLATILE MATTER
7.1 Boil 2 g of the sample 2 min with 25 mL of water, let 8. Procedure
settle, and decant the supernatant liquid. Similarly, boil the
8.1 Determine moisture and other volatile matter in accor-
residue with 25 mL of ethyl alcohol (absolute or 95 %) and
dance with Test Method A of Test Methods D 280.
decant as before. Likewise boil with 25 mL of chloroform and
again decant. If any one of the above solutions is colored, MATTER SOLUBLE IN WATER
organic colors are present. If all solutions remain colorless, 9. Procedure
organic colors are presumably absent. The presence of organic
9.1 Place 2.5 g of the sample in a graduated 250-mL flask.
colors resistant to the above reagents is unlikely, but may be
6
Reference may be made to the following: Payne, H. F., “Organic Coatings
Technology,” Vol II, John Wiley & Sons, Inc., New York, NY, 1961.

2
 D 126
Add 100 mL of water and boil for 5 min. Cool, dilute to exactly chromium is reduced, as indicated by a green color. Filter if
250 mL, mix, and allow to settle. Filter the supernatant liquid any insoluble residue is present, retaining the filtrate and
through a dry paper and discard the first 20 mL. Evaporate 100 washings for the determination. Add NH4OH (sp gr 0.90) to
mL of the clear filtrate to dryness in a weighed dish, heat for 1 this solution until a faint precipitate begins to form; then add 5
h at 105 to 110°C, cool, and weigh. mL of HCl (sp gr 1.19) slowly, dilute to 500 mL, and pass a
9.2 Calculation—Calculate the % of matter soluble in water rapid current of H2S into the solution until precipitation is
as follows: complete. Settle, filter, and wash with water containing H2S.
Matter soluble in water, % 5 ~R3 2.5 3 100!/S (1) 12.2 Rinse the precipitate from the filter (Note 5) into a
beaker containing 25 mL of HNO3(1+3) and boil until all PbS
where: has dissolved. Add 10 mL of H2SO4(1+1) and evaporate to
R = weight of residue, and strong fumes of SO3. Cool and add 50 mL of water and 50 mL
S = specimen weight, g. of ethyl alcohol (95 %) (Note 6). Let stand 1 h; then filter on
a tarred Gooch crucible. Wash with ethyl alcohol (95 %), dry,
LEAD CHROMATE7
ignite at 500 to 600°C, and weigh as PbSO4.
10. Reagents NOTE 5—If a trace of sulfide remains on the paper, the stained portion
10.1 Dissolving Solution—Saturate 1 L of water with NaCl. of the paper may be separately treated with bromine water, the paper
Filter. Add to the filtered solution 150 mL of water and 100 mL filtered off, and the filtrate added to the body of the solution.
NOTE 6—Any sulfur remaining from decomposition of the sulfides may
of HCl (sp gr 1.19). be mechanically removed as a globule of solidified sulfur at this point.
10.2 Ferrous Sulfate, Standard Solution (0.3 N)—Dissolve
86 g of FeSO4 · 7H2O in 500 mL of water to which 30 mL of SULFATE7
H2SO4 (sp gr 1.84) has been added with constant stirring.
Dilute to 1 L and standardize not more than 6 h before use by 13. Reagents
potentiometric titration against 0.7-g portions of K2Cr2O7. 13.1 Barium Chloride Solution—Dissolve 117 g of BaCl2 ·
2H2O in water and dilute to 1 L.
11. Procedure 13.2 Dissolving Solution—See 10.1.
11.1 Dissolve 1 g of the sample in 150 mL of the dissolving 13.3 Sodium Carbonate Solution —(saturated)—Prepare a
solution. Agitate for 10 to 15 min, keeping the solution cold solution containing excess Na2CO3 at laboratory temperature,
until dissolution is complete (Note 4). If dissolution is not and free of SO4. Decant the clear solution for use as required.
complete, filter through fine grade filter paper and wash with
three 10-mL portions of cold dissolving solution. Add 10 mL of 14. Procedure
HClO4 (70 %), dilute to 250 mL, and titrate potentiometrically 14.1 Digest 1.25 g of the sample with 100 mL of dissolving
with FeSO4 solution. solution at 100°C for 5 min. Add 25 mL of glacial acetic acid
NOTE 4—Incomplete solution of the pigment is evidence of the possible
and 15 mL of ethyl alcohol and heat gently for 10 min to
presence of barium sulfate, silica, silicates, or other acid-insoluble reduce chromium, as indicated by the green color of the
extenders (see Section 18). Some chrome yellows may contain organic solution. Cool. Neutralize with saturated Na2CO3 solution and
addition agents and will give a turbid solution at this point. add a slight excess. Transfer to a 250-mL volumetric flask,
Newer chemically resistant-type lead chromate type pigments (silica dilute to the mark with distilled water, and mix. Filter without
encapsulated) cannot be decomposed by the procedures described in this washing through a dry filter paper, discarding the first 10 to 15
method. Pigments of this type may require treatment with strong alkali
mL.
hydroxide or hydrofluoric acid.
Also, if trivalent antimony has been used in manufacturing the product, 14.2 Take a 200-mL aliquot of the filtrate, neutralize with
pentavalent antimony may be present which would interfere in the HCl (1+1), and add 10 mL excess. Heat to boiling and boil for
determination of lead chromate. 5 min. To the gently boiling solution, add 15 mL of BaCl2
11.2 Alternatively, the solution may be reduced by a known solution dropwise with constant stirring. Digest on a steam
excess of FeSO4 solution and back-titrated with KMnO4 bath for 2 h. Filter through an ignited tarred Gooch crucible,
solution in the presence of MnSO4, or excess KI may be added wash with HCl (1+99), and finally with hot water. Dry at 105
and the liberated iodine titrated with Na2S2O3 solution, using to 110°C, ignite at 900°C, and weigh.
starch indicator. The iodine liberation method is not applicable CARBON DIOXIDE7
in the presence of molybdenum.
15. Procedure
TOTAL LEAD7
15.1 Determine CO2 by the evolution method on 2.5 g of the
12. Procedure sample, using dilute HNO3 free of NO or NO2 and absorbing
12.1 Dissolve 0.5 g of sample as described in Section 11. the CO2 in soda lime or in KOH solution.
Add 5 mL of ethyl alcohol (95 % or absolute) and boil until the MOLYBDENUM7

7
16. Reagents
Sections 23 and 24 under “Calculation of Substances Other than Insoluble Lead
Compounds” should be read carefully before proceeding with the analyses described 16.1 Ferric Sulfate Solution—Dissolve 20 g of Fe2(SO4)3 ·
in Sections 10 to 22. (NH4)2SO4 · 24H2O in 200 mL of water to which has been

3
 D 126
added 50 mL of H2SO4 (sp gr 1.84) and 20 mL of H3PO4 Section 10, as follows:
(85 %), and dilute to 1 L. A. Extenders Soluble in Dissolving Solution—Calcium sul-
16.2 Jones Reductor—The reductor shall contain at least a fate (gypsum), calcium carbonate (whiting), and magnesium
35-cm column of amalgamated zinc, prepared by shaking 20 to carbonate.
30-mesh zinc free of iron or carbon with HgCl2 solution (20 B. Extenders Insoluble in Dissolving Solution—Silica, mag-
g/L) in sufficient quantity to produce an amalgam containing 1 nesium silicate, and clay (Note 7).
to 5 % of mercury, and supported by a suitable inert pad of 18.2 Extenders of group A may be present if the analysis
asbestos, glass wool, or other inert material. shows sulfates and carbonates to be in the pigment, and are
16.3 Potassium Permanganate, Standard Solution (0.1 absent if sulfate and carbonate are absent. Since the latter
N)—Dissolve 3.16 g of KMnO4 in water and dilute to 1 L. Let situation rarely exists, it is advisable to test for the presence of
stand 8 to 14 days, siphon off the clear solution (or filter calcium and magnesium to determine if extenders are present.
through a medium porosity fritted disk), and standardize Extenders of group B are recognized as an insoluble residue
against the National Bureau of Standards standard sample No. following acid solution of the pigment, and may be determined
40 of sodium oxalate (Na2C2O4) as follows: In a 400-mL quantitatively if desired, by the method described in Section
beaker dissolve 0.2500 to 0.3000 g of the Bureau of Standards 31. Extenders of group A, if present, may affect the calculation
sodium oxalate in 250 mL of hot water (80 to 90°C) and add 15 of insoluble lead compounds as given in Section 23. Their
mL of H2SO4 (1+1). Titrate at once with KMnO4 solution, qualitative or quantitative estimation may be necessary.
stirring the liquid vigorously and continuously. The KMnO4
NOTE 7—Some lead chromates may contain zirconium or titanium
must not be added more rapidly than 10 to 15 mL/min, and the compounds, some of which are insoluble in the dissolving solution, but are
last 0.5 to 1 mL must be added dropwise with particular care to not to be considered as extenders, since they have been added to improve
allow each drop to be fully decolorized before the next is the properties of the pigment.
introduced. The solution shall not be below 60°C by the time
the end point has been reached. (More rapid cooling may be Qualitative Detection of Extenders of Group A
prevented by allowing the beaker to stand on a small asbestos-
19. Reagents
covered hot plate during the titration. The use of a small
thermometer (non-mercury type) as a stirring rod is most 19.1 Ammonium Phosphate Solution—Dissolve 100 g of
convenient.) Keep the KMnO4 solution in a glass-stoppered (NH4)2HPO4 in water and dilute to 1 L.
bottle painted black to keep out light, or in a brown glass bottle
stored in a dark place. 20. Procedure
20.1 Dissolve 1 g of the sample as described in Section 11.
17. Procedure Add 5 mL of ethyl alcohol (95 % or absolute) and boil until the
17.1 Dissolve 1 g of the sample as described in Section 11. chromium is reduced. An insoluble residue at this point denotes
Add 5 mL of ethyl alcohol (95 % or absolute) and boil until the presence of extenders of Group B. Filter if necessary and
chromium is reduced. Filter if any insoluble residue is present, wash well.
retaining the filtrate and washings. Add NH4OH (sp gr 0.90) 20.2 To the filtrate, add NH4OH (1+4) until just ammonia-
cautiously until a faint precipitate begins to form, then add 15 cal, boil 5 min, and allow to digest in a warm place until the
mL of H2SO4 (sp gr 1.84) and dilute to 300 mL. Heat to precipitate has coagulated. Filter, washing well with hot water
boiling, pass in a rapid stream of H2S for 15 min, and dilute and reserving the filtrate. Dissolve the precipitate on the filter
with 300 mL of hot water. Pass in H2S for 10 min, boil for 3 with HCl (1+1), washing back into the original beaker.
min, and cool. Pass in H2S for 10 min, and let stand at room Reprecipitate, filter, and wash as before.
temperature for 1 h. Filter and wash with H2SO4 (1+99) 20.3 Combine the washings, make just acid with HCl (1+1),
saturated with H2S. and evaporate to a volume of about 250 mL. Add 50 mL of
17.2 Rinse the sulfide precipitate into the original beaker (NH4)2HPO4 solution, cool, and add 50 mL of NH4OH (sp gr
and add 20 mL of HNO3 (sp gr 1.42) and 5 mL of H2SO4(sp gr 0.90). Allow to stand overnight. A precipitate indicates the
1.84) (see Note 5). Cover and heat to fumes. Cool, add 10 mL presence of extenders of Group A.
of HNO3 (sp gr 1.42), and again fume. Repeat this operation if
necessary until a light-colored solution is obtained. Wash the Quantitative Determination of Extenders of
cover and inside of the beaker and fume again to remove all Group A
HNO3. Dilute to 200 mL and add NH4OH (1+4) until neutral;
then add 10 mL of H2SO4(sp gr 1.84). 21. Reagents
17.3 Cool the solution and reduce by passing through a 21.1 Ammonium Oxalate Solution—Dissolve 30 g of am-
Jones reductor at a rate not exceeding 100 mL/min, collecting monium oxalate in water and dilute to 1 L.
the effluent under 200 mL of Fe2(SO4)3 solution. Titrate with 21.2 Ammonium Phosphate Solution—See Section 19.
KMnO4 solution. A blank determination should also be made.
22. Procedure
EXTENDERS7
22.1 If the sample is a chrome yellow or orange use the
18. General Considerations procedure given in Section 14 for dissolving and reducing
18.1 Extenders fall into two groups, depending on their chromium. For other chromium pigments heat gently 2 g of
solubility or insolubility in the dissolving solution described in sample in a porcelain dish without ignition until iron blue, if

4
 D 126
present, is just decomposed. Transfer to a beaker and dissolve D 5 excess PbO, % 5 C – ~0.6906 B 1 0.6078 A! (7)
the lead salts in 150 mL of dissolving solution as described in 23.5 Calculate the sulfate as SO3 from the analysis of
Section 11. Section 14 as follows:
22.2 Add 20 ml of HCl (sp gr 1.19) and digest 1 h at 100°C.
E 5 SO3, % 5 grams of BaSO4 3 34.3 (8)
Dilute to 300 mL, filter and wash thoroughly. Add NH4OH
(1+4) to the filtrate and washings until just ammoniacal, boil 5 23.5.1 If E is equal to or greater than 0.3587 D, the % of
min and allow to digest in a warm place until the hydroxides PbSO4 equals 1.3587 D, and the % total insoluble lead
and hydrous oxides are coagulated. Filter, washing well with compounds equals A + B + 1.3587 D.
diluted water and reserve the filtrate. Redissolve the precipitate 23.5.2 If E is less than 0.3587 D, the percentage of PbSO4
with HCl (1+1) washing back into the original beaker. Repre- equals 3.788 E, and a new excess of PbO is calculated as
cipitate, filter and wash as before. Combine the washings with follows:
the original filtrate and add 50 mL of ammonium oxalate F 5 Excess PbO, % 5 D 2 2.788 E (9)
solution. Filter off the CaC2O4 precipitate on quantitative 23.6 Calculate the percent of CO2 from the analysis of
paper. Transfer to a tarred crucible, ash, ignite at 1300°C, cool Section 15 as follows:
in a desiccator, and weigh as CaO. Alternatively, the washed
precipitate may be dissolved in H2SO4(1+1) and the resulting G 5 CO2, % 5 grams of CO2 3 40 (10)
solution titrated hot with 0.1 N KMnO4 solution, as described 23.6.1 If G is equal to or greater than 0.1314 F, the percent
in the Procedure section under Calcium in Test Methods D 521. of basic lead carbonate (2 PbCO3 · Pb(OH)2) is 1.1584 F and
22.3 Make the filtrate from the calcium determination the percent of total insoluble lead compounds is A + B + 3.788
slightly acid with HCl (1+1) and evaporate to 250 mL volume. E + 1.1584 F.
Add 50 mL of (NH4)2HPO4 solution, cool, and add 50 mL of 23.6.2 If G is appreciably in excess, extenders are probably
NH4OH (sp gr 0.90). Allow to stand overnight. Filter on present. If G is less than 0.1314 F, the percent of 2
suitable quantitative paper, wash with NH4OH (1+19), ignite in PbCO3·Pb(OH)2 is 8.813 G and the excess PbO is:
a platinum crucible at 1050°C for 1 h and weigh. Care must be H 5 Excess PbO, % 5 F 2 7.608 G (11)
taken to char the paper slowly before igniting.
22.4 Calculation—Calculate the percent of extenders (as 23.6.2.1 The percent of total insoluble lead compounds is
oxides) as follows: A + B + 3.788 E + 8.813 G + H.
Calcium oxide, % 5 weight of CaO 3 50 (2) 24. Calculations Where Extenders Are Present
24.1 If extenders are present, calculate the CO2 equivalent
Magnesium oxide, % 5 weight of Mg2P2O7 3 18.11 (3)
as follows:
The calculation of the amount of extenders as carbonates or I 5 CO2 equivalent of extenders (12)
sulfates is described in Section 24.
5 CaO, % 3 0.786 1 MgO, % 3 1.100
CALCULATION OF SUBSTANCES OTHER THAN
24.2 If I is less than G, use G − I as the net CO2 for purposes
INSOLUBLE LEAD COMPOUNDS
calculating the 2PbCO3·Pb(OH)2 content of the pigment.
23. Calculations Where Extenders Are Absent Total extenders 5 CaO, % 1 MgO, % 1 I (13)
23.1 “Insoluble lead compounds” in chrome yellow and 24.3 If I is greater than G, some of the extender is present as
chrome orange may consist of PbCrO4, PbSO4, 2PbCO3 · CaSO4(Note 8). Calculate the total percent of extenders as
Pb(OH)2, PbO, or PbMoO4. The first two are characteristic of follows:
the chrome yellows, the first, third, and fourth of the basic
chrome oranges, and the first, second, and last of molybdate J 5 CO2 equivalent of MgO 5 MgO % 3 1.100 (14)
oranges. For purpose of determining conformance with speci-
fication requirements, where “insoluble lead compounds” are K 5 CO2 present as CaCO3 5 G – J (15)
defined as above, make the following calculations if extenders
are absent: CaCO3, % 5 2.73 K (16)
23.2 If molybdenum is present, calculate the percent of
PbMoO4 from the titration of Section 17 as follows: L 5 CaO present as sulfate, % 5 CaO, % 6 1.27 K (17)
A 5 PbMoO4, % 5 mL titration 3 normality of KMnO4 3 12.24
(4) CaSO4, % 5 2.43 L (18)
23.3 Calculate the percent of PbCrO4 from the titration of
Section 11 as follows: SO3 combined as CaSO4, % 5 1.43 L (19)

B 5 PbCrO4, % 5 mL titration 3 normality of FeSO4 3 10.77 (5) 24.3.1 E − 1.43 L equals the net SO3 to be used for
calculating the PbSO4 content of the pigment. If I is greater
23.4 Calculate the percent of total lead as oxide and the
than G, no calculation of 2PbCO3 · Pb(OH)2 is necessary, and
percent of excess PbO from the analysis of Section 12 as
the excess PbO is given by F.
follows:
Total extenders, % 5 2.100 3 MgO, % 1 2.73 K 1 2.43 L (20)
C 5 PbO, % 5 grams of PbSO4 3 147.2 (6)
NOTE 8—It is impractical to detect by chemical means whether a

5
 D 126
pigment contains CaCO3 and PbSO4, or CaSO4 and 2PbCO3 · Pb(OH)2.
This calculation assumes the former as more probable.

PURE CHROME GREEN AND REDUCED CHROME GREEN

ORGANIC COLORS AND LAKES is not clear after 5 min boiling, add 5 mL of additional HCl
(1+4), and repeat until a clear solution is obtained. Cool and
25. Procedure titrate with FeSO4 solution on a potentiometric apparatus; or
25.1 Determine organic colors and lakes in accordance with alternatively, add a measured excess of FeSO4 and back-titrate
Section 7. with KMnO4 solution in the presence of MnSO4.

MOISTURE AND OTHER VOLATILE MATTER BARIUM SULFATE AND INSOLUBLE SILICEOUS
MATERIAL8
26. Procedure
26.1 Determine moisture and other volatile matter in accor- 31. Procedure
dance with Section 8. 31.1 Heat gently 1 g of sample in a porcelain dish without
ignition until the iron blue is just decomposed. Transfer to a
MATTER SOLUBLE IN WATER beaker and dissolve the lead salts as described in Section 11,
warming if necessary. Filter through a tared Gooch crucible,
27. Procedure
wash thoroughly, ignite at 600 to 800°C, and weigh.
27.1 Determine matter soluble in water in accordance with 31.2 Calculation—Calculate the percent of BaSO4 and
Section 9. insoluble siliceous material as follows:
IRON BLUE BaSO4 and insoluble siliceous material, % (22)
5 weight of precipitate 3 100
28. Procedure
28.1 Determine the total nitrogen (by the Kjeldahl-Gunning TOTAL LEAD
method) (Note 9) on 1 g of the sample, adding 2 g of FeSO4 ·
32. Procedure
7H2O before digestion for at least 21⁄2 h.
32.1 Determine total lead on the filtrate from the determi-
NOTE 9—For further details refer to Test Method D 1013. nation of BaSO4 and insoluble matter (Section 31) in accor-
28.2 Calculation—Calculate the percent of iron blue as dance with the directions of Section 12.
follows:
SULFATE
Iron blue, % 5 nitrogen, % 3 3.4 (21)
NOTE 10—Qualitative tests may be made for other nitrogen-containing 33. Procedure
blue pigments.
33.1 After decomposition of the iron blue in 1.25 g of
LEAD CHROMATE sample as described in Section 31, digest the residue with 20
mL of HCl (sp gr 1.19) at 100°C until solution is complete.
29. Reagents Add 300 mL of water and heat to boiling. Filter and wash
29.1 Ferrous Sulfate, Standard Solution (0.3 N)—See 10.2. thoroughly. Determine sulfate on the filtrate and washings as
29.2 Potassium Permanganate Standard Solution (0.1 N)— described in Section 14.
Prepare as described in 16.3. Standardization is unnecessary
CALCIUM OXIDE SOLUBLE IN ACID
except for the alternative procedure given in Section 30.
34. Reagents
30. Procedure
34.1 Ammonium Oxalate Solution—See 21.1.
30.1 Mix thoroughly 1 g of sample with at least 10 g of
Na2O2 in a 30-mL pure iron crucible. Heat gently until the 35. Procedure
fusion is complete; then heat strongly, rotating the crucible
with iron tongs (not Nichrome or chromium plate) for a few 35.1 Decompose 2 g of sample as described in Section 31.
minutes to ensure complete fusion. Allow to cool; then transfer Add 20 mL of HCl (sp gr 1.19) and proceed in accordance with
the crucible and cover to a beaker containing 250 mL of water. 21.1 to the end of the calcium determination.
When the action has ceased, rinse and remove the crucible and 35.2 Calculation—Calculate the percent of CaO soluble in
cover, and boil for at least 10 min to destroy excess peroxide. acid as follows:
Make just acid with H2SO4 (1+1) and add about 35 mL in CaO soluble in acid, % 5 grams CaO 3 50 (23)
excess. Add 2.5 mL of 0.1 N KMnO4 solution and heat to
boiling. Add 10 mL of HCl (1+4) and boil to reduce manganese
and lead as indicated by clearing of the solution. If the solution 8
See Note 7 of Section 18.

6
 D 126
EXTENDERS CALCULATION OF INSOLUBLE LEAD
COMPOUNDS
36. Procedure
36.1 The method described in Sections 31, 34, and 35 37. Procedure
suffices for the detection and estimation of all common
extenders except MgCO3. This may be tested for the filtrate 37.1 The insoluble lead compounds may be calculated by
from the CaO determination by the method described in the methods of Sections 23 and 24.
Section 22.

CHROMIUM OXIDE GREEN

ORGANIC COLORS AND LAKES 41.2 Calculation—Calculate the percent of chromium as

Cr2O3 as follows:
38. Procedure
Cr2O3, % 5 mL titration 3 normality of FeSO4 3 63.34 (24)
38.1 Determine organic colors and lakes in accordance with
Section 7. 42. Precision and Bias
MOISTURE AND OTHER VOLATILE MATTER 42.1 Data are not available to determine the precision and
39. Procedure bias of these test methods. There are no plans at present to
obtain such data.
39.1 Determine in accordance with Section 8.
MATTER SOLUBLE IN WATER 43. Keywords

40. Procedure 43.1 chromium oxide green pigment; green pigment con-
taining lead chromate and chromium oxide; lead chromate
40.1 Determine in accordance with Section 9. pigment; lead containing pigment; molybdate pigment; orange
TOTAL CHROMIUM AS CHROMIUM OXIDE pigment containing lead chromate and chromium oxide; yellow
pigment containing lead chromate and chromium oxide
41. Procedure
41.1 Using 0.4 g of the sample proceed as in Section 30.

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