Printed on: Wed Jan 18 2023, 02:29:08 AM(EST) Status: Not Yet Official on 18-Jan-2023 DocId: GUID-D6ED6363-05B2-45EC-8B28-684A0D5BC4B6_7_en-US

Printed by: Rock Pharma Official Date: 01-Jun-2023 Document Type: USP & DS & NF @2023 USPC
Do Not Distribute DOI Ref: 73wrp DOI: https://doi.org/10.31003/USPNF_M12005_07_01
1

IMPURITIES
Anhydrous Dibasic Calcium Phosphate • CARBONATE
Portions of this monograph that are national USP text, and are Sample: 1.0 g of Anhydrous Dibasic Calcium Phosphate
not part of the harmonized text, are marked with symbols Analysis: Mix the Sample with 5 mL of carbon dioxide-free
(◆◆) to specify this fact. water, and immediately add 2 mL of hydrochloric acid.
Acceptance criteria: No effervescence occurs.
CaHPO4 136.06 • CHLORIDE AND SULFATE á221ñ, Chloride
Phosphoric acid, calcium salt (1:1); Standard solution: To 0.70 mL of 0.01 N hydrochloric acid,
Calcium phosphate (1:1) CAS RN®: 7757-93-9. add 6 mL of diluted nitric acid, and dilute with water to
50 mL.
DEFINITION Sample solution: To 0.20 g of Anhydrous Dibasic Calcium
Anhydrous Dibasic Calcium Phosphate contains NLT 97.5% Phosphate, add 20 mL of water and 13 mL of diluted nitric
and NMT 102.5% of anhydrous dibasic calcium phosphate acid, and warm gently, if necessary, to completely dissolve.

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(CaHPO4). Dilute with water to 100 mL, and filter if necessary. Use
IDENTIFICATION 50 mL of the solution as Sample solution.
• A. Analysis
Sample: 0.1 g of Anhydrous Dibasic Calcium Phosphate Samples: Standard solution and Sample solution
Analysis: Dissolve the Sample by warming in 10 mL of 2 N Add 1 mL of silver nitrate TS to the Sample solution and

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hydrochloric acid. Add 2.5 mL of ammonia TS dropwise, the Standard solution, respectively. Mix well, and allow
with shaking, and then add 5 mL of ammonium oxalate TS. to stand for 5 min protecting from direct sunlight.
Acceptance criteria: A white precipitate is formed. Compare the opalescence developed in both solutions
• B. against a black background by viewing downward or
Sample: 0.1 g of Anhydrous Dibasic Calcium Phosphate transversely.

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Analysis: Dissolve the Sample in 5 mL of diluted nitric acid. Acceptance criteria: The opalescence of the Sample solution
Warm the solution to 70°, and add 2 mL of 10% does not exceed that of the Standard solution (NMT
ammonium molybdate solution (freshly prepared). 0.25%).
Acceptance criteria: A yellow precipitate of ammonium • CHLORIDE AND SULFATE á221ñ, Sulfate
phosphomolybdate is formed. Standard solution: To 1.0 mL of 0.010 N sulfuric acid, add
1 mL of diluted hydrochloric acid, and dilute with water to
ASSAY
O 50 mL.
• PROCEDURE Sample solution: To 0.5 g of Anhydrous Dibasic Calcium
Buffer: Dissolve 53.5 g of ammonium chloride with Phosphate, add 5 mL of water and 5 mL of diluted
sufficient water in a 1000-mL volumetric flask. Add 570 mL hydrochloric acid, and warm gently, if necessary, to
of ammonia water, stronger, and dilute with water to completely dissolve. Dilute with water to 100 mL, and filter
volume. The pH of this solution is 10.7. if necessary. To 20 mL of the solution add 1 mL of diluted
Sample solution: Transfer 400 mg of Anhydrous Dibasic hydrochloric acid, and dilute with water to 50 mL.
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Calcium Phosphate to a 200-mL volumetric flask. Dissolve Analysis
in 12 mL of diluted hydrochloric acid with the aid of gentle Samples: Standard solution and Sample solution
heat, if necessary, and dilute with water to volume. Add 2 mL of barium chloride TS to the Sample solution and
Blank: 20 mL of water containing 1.2 mL of diluted the Standard solution, respectively. Mix well, and allow
B

hydrochloric acid to stand for 10 min. Compare the white turbidity

Titrimetric system produced in both solutions against a black background
(See Titrimetry á541ñ.) by viewing downward or transversely.
Mode: Residual titration Acceptance criteria: The turbidity of the Sample solution
Titrant: 0.02 M edetate disodium VS does not exceed that of the Standard solution (NMT 0.5%).
Back-titrant: 0.02 M zinc sulfate VS
To

Endpoint detection: Visual Change to read:

Analysis: To 20.0 mL of the Sample solution add 25.0 mL of
Titrant, 50 mL of water, and 5 mL of Buffer. Add 25 mg of • ARSENIC á211ñ, Procedures, Procedure 1▲ (CN 1-Jun-2023)
◆ ▲

eriochrome black T–sodium chloride indicator. Titrate the Test preparation: 1.0 g in 25 mL of 3 N hydrochloric acid,
excess Titrant with the Back-titrant. Perform a Blank diluted with water to 55 mL. Omit the addition of 20 mL of
determination in the same manner. 7 N sulfuric acid specified in Procedure.
Calculate the percentage of anhydrous dibasic calcium Acceptance criteria: NMT 3 µg/g◆
phosphate (CaHPO4) in the sample taken: • BARIUM
Sample: 0.5 g Anhydrous Dibasic Calcium Phosphate
Result = {[(VB − VS) × M × F]/W} × 100 Analysis: Heat the Sample to boiling with 10 mL of water,
and add 1 mL of hydrochloric acid dropwise, stirring after
VB = Back-titrant volume consumed by the Blank each addition. Allow to cool, and filter if necessary. To the
(mL) filtrate add 2 mL of potassium sulfate TS.
VS = Back-titrant volume consumed by the Sample Acceptance criteria: No turbidity is produced within
(mL) 10 min.
M = actual molarity of the Back-titrant (mmol/mL) • LIMIT OF ACID-INSOLUBLE SUBSTANCES
F = equivalency factor, 136.06 mg/mmol Sample solution: Dissolve 5.0 g in a mixture of 40 mL of
W = sample weight (mg) in 20.0 mL of the Sample water and 10 mL of hydrochloric acid by boiling gently for
solution 5 min.
Analysis: After cooling, collect the insoluble substance on
Acceptance criteria: 97.5%–102.5% ashless filter paper, and wash with water until the last
washing does not give a reaction for chloride (no turbidity
results from the addition of silver nitrate TS). Ignite to

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Printed on: Wed Jan 18 2023, 02:29:08 AM(EST) Status: Not Yet Official on 18-Jan-2023 DocId: GUID-D6ED6363-05B2-45EC-8B28-684A0D5BC4B6_7_en-US
Printed by: Rock Pharma Official Date: 01-Jun-2023 Document Type: USP & DS & NF @2023 USPC
Do Not Distribute DOI Ref: 73wrp DOI: https://doi.org/10.31003/USPNF_M12005_07_01
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completely incinerate the residue and the ashless filter addition. Plot the logarithms of the cumulative fluoride
paper at 600 ± 50°. ion concentrations (0.1, 0.2, 0.5, and 1.0 µg/mL) versus
Acceptance criteria: The weight of the residue does not potential in millivolts.
exceed 10 mg (NMT 0.2%). Rinse and dry the electrodes, insert them into the Sample
• ◆LIMIT OF FLUORIDE solution, stir for 5 min, and read the potential in
[NOTE—Prepare and store all solutions in plastic millivolts. From the measured potential and the Standard
containers.] response line determine the concentration (C), in µg/mL,
Buffer solution: 294 mg/mL of sodium citrate dihydrate in of fluoride ion in the Sample solution.
water Calculate the content of fluoride in ppm in the portion of
Standard stock solution: 1.1052 mg/mL of USP Sodium Anhydrous Dibasic Calcium Phosphate taken:
Fluoride RS in water
Standard solution: Transfer 20.0 mL of Standard stock Result = (V × C)/W
solution to a 100-mL volumetric flask containing 50.0 mL of

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Buffer solution, dilute with water to volume, and mix. Each V = Sample solution volume (mL)
milliliter of this solution contains 100 µg of fluoride ion. C = concentration of fluoride ion, determined from
Sample solution: Transfer 2.0 g of Anhydrous Dibasic the Standard response line, in the Sample solution
Calcium Phosphate to a beaker containing a plastic-coated (µg/mL)
stirring bar. Add 20 mL of water and 2.0 mL of hydrochloric W = weight of Anhydrous Dibasic Calcium Phosphate

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acid, and stir until dissolved. Add 50.0 mL of Buffer solution taken to prepare the Sample solution (g)
and sufficient water to make 100 mL.
Electrode system: Use a fluoride-specific ion-indicating Acceptance criteria: NMT 50 ppm◆
electrode and a silver–silver chloride reference electrode SPECIFIC TESTS
connected to a pH meter capable of measuring potentials • LOSS ON IGNITION á733ñ

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with a minimum reproducibility of ±0.2 mV (see pH á791ñ). Sample: 1 g of Anhydrous Dibasic Calcium Phosphate
Analysis Analysis: Ignite the Sample at 800°–825° to constant
Samples: Standard solution and Sample solution weight.
Standard response line: Transfer 50.0 mL of Buffer Acceptance criteria: 6.6%–8.7%
solution and 2.0 mL of hydrochloric acid to a beaker, and
add water to make 100 mL. Add a plastic-coated stirring ADDITIONAL REQUIREMENTS
• ◆PACKAGING AND STORAGE: Preserve in well-closed
O
bar, insert the electrodes into the solution, stir for 15 min,
and read the potential in millivolts. Continue stirring, and containers. No storage requirements specified.◆
at 5-min intervals add 100, 100, 300, and 500 µL of • USP REFERENCE STANDARDS á11ñ
Standard solution, reading the potential 5 min after each USP Sodium Fluoride RS
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B
To

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