Monograph pubs.acs.org/doi/book/10.1021/acsreagents
Lead Carbonate Part 4, Monographs for Reagent Chemicals: General Descriptions, Specifications, and Tests eISBN: 9780841230460 Tom Tyner Chair, ACS Committee on Analytical Reagents James Francis Secretary, ACS Committee on Analytical Reagents
ABSTRACT This monograph for Lead Carbonate provides, in addition to common physical constants, a general description including typical appearance, applications, change in state (approximate), and aqueous solubility. The monograph also details the following specifications and corresponding tests for verifying that a substance meets ACS Reagent Grade specifications including: Insoluble in Dilute Acetic Acid, Chloride, Nitrate, Nitrite, Cadmium, Calcium, Iron, Potassium, Sodium, and Zinc.
PbCO3 (normal) (PbCO3)2Pb(OH)2 (basic)
Formula Wt 267.22 Formula Wt 775.66
CAS No. 598-63-0 CAS No. 1344-36-1
Note: This specification applies to both the normal lead carbonate and the basic lead carbonate.
GENERAL DESCRIPTION Typical appearance . . . . . . . . Applications . . . . . . . . . . . . . Change in state (approximate) . Aqueous solubility . . . . . . . . .
. . . .
. . . .
. . . .
. . . .
. . . .
. . . .
. . . .
. . . .
. . . .
. . . .
. . . .
heavy white solid preparation of lead standard solutions decomposes at 400 °C insoluble
. . . . . .
Maximum Allowable 0.02% 0.002% Passes test 0.002% 0.01% 0.005%
SPECIFICATIONS Insoluble in dilute acetic acid Chloride (Cl) . . . . . . . . . . . Nitrate and nitrite (as NO3) . . Cadmium (Cd) . . . . . . . . . . Calcium (Ca) . . . . . . . . . . . Iron (Fe) . . . . . . . . . . . . . .
. . . . . .
. . . . . .
. . . . . .
. . . . . .
. . . . . .
. . . . . .
. . . . . .
. . . . . .
. . . . . .
. . . . . .
. . . . . .
© 2017 American Chemical Society
A
DOI:10.1021/acsreagents.4187 ACS Reagent Chemicals, Part 4
ACS Reagent Chemicals
Monograph
pubs.acs.org/doi/book/10.1021/acsreagents
Potassium (K) . . . . . . . . . . . . . . . . . . . . . . . 0.02% Sodium (Na) . . . . . . . . . . . . . . . . . . . . . . . . 0.05% Zinc (Zn) . . . . . . . . . . . . . . . . . . . . . . . . . . 0.003%
TESTS Insoluble in Dilute Acetic Acid Digest 5.0 g in 50 mL of water plus 7 mL of glacial acetic acid in a covered beaker on a hot plate (~100 °C) for 1 h. Filter through a tared, preconditioned filtering crucible, wash thoroughly with dilute acetic acid (2:98), and dry at 105 °C.
Chloride [Part 2: Colorimetry and Turbidimetry; Chloride]. Dissolve 1.0 g in 20 mL of 10% nitric acid reagent solution, filter if necessary through a chloride-free filter, and dilute with water to 50 mL. Use 25 mL of this solution.
Nitrate and Nitrite [Part 2: Colorimetry and Turbidimetry; Nitrate; Procedure for Nitrate, Method 1 (Brucine Sulfate)].
For the Determination of Nitrate and Nitrite
S a m p l e S o l u t i o n A . Dissolve 0.20 g in 1 mL of water and 8 mL of dilute acetic acid (1:7) by heating on a hot plate (~100 °C). Add 20 mL of nitrate-free sulfuric acid (2:1), cool, centrifuge, and decant the liquid portion into a 200 mm test tube. Dilute to 50 mL with brucine sulfate reagent solution. C o n t r o l S o l u t i o n B . Dissolve 0.20 g in 8 mL of dilute acetic acid (1:7) and 1 mL of nitrate ion (NO3) standard solution by heating on a hot plate (~100 °C). Add 20 mL of nitrate-free sulfuric acid (2:1), cool, centrifuge, and decant the liquid portion into a 200 mm test tube. Dilute to 50 mL with brucine sulfate reagent solution.
Continue with the procedure, starting with the preparation of blank solution C. (Limit about 0.005%.)
Cadmium, Calcium, Iron, Potassium, Sodium, and Zinc (By flame AAS, [Part 2: Trace and Ultratrace Elemental Analysis; Atomic Absorption Spectroscopy; Analysis; Procedure for Flame AAS]).
For the Determination of Cadmium, Calcium, Iron, Potassium, Sodium, and Zinc
S a m p l e S t o c k S o l u t i o n . Dissolve 10.0 g in 50 mL of water and sufficient nitric acid to achieve complete dissolution. Transfer the solution to a 100 mL volumetric flask, and dilute to the mark with water (1 mL = 0.1 g).
© 2017 American Chemical Society
B
DOI:10.1021/acsreagents.4187 ACS Reagent Chemicals, Part 4
ACS Reagent Chemicals
Monograph
pubs.acs.org/doi/book/10.1021/acsreagents
For the Determination of Cadmium, Calcium, Iron, Potassium, Sodium, and Zinc
Element
Wavelength (nm)
Sample Wt (g)
Standard Added (mg)
Flame Type*
Background Correction
Cd
228.8
1.0
0.02; 0.04
A/A
Yes
Ca
422.7
0.40
0.02; 0.04
N/A
No
Fe
248.3
1.0
0.05; 0.10
A/A
Yes
K
766.5
0.20
0.02; 0.04
A/A
No
Na
589.0
0.04
0.01; 0.02
A/A
No
Zn
213.9
0.40
0.01; 0.02
A/A
Yes
*A/A is air/acetylene; N/A is nitrous oxide/acetylene.
© 2017 American Chemical Society
C
DOI:10.1021/acsreagents.4187 ACS Reagent Chemicals, Part 4
