Printed on: Fri Jan 05 2024, [Link] PM(EST) Status: Currently Official on 06-Jan-2024 DocId: GUID-C59E1D6A-1A19-46B9-921B-2E62997EE426_4_en-US

Printed by: USP NF Official Date: Official as of 01-May-2020 Document Type: NF @2024 USPC
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rS = peak response of benzaldehyde from the

Benzaldehyde Standard solution
CS = concentration of USP Benzaldehyde RS in the
Standard solution (mg/mL)
CU = concentration of Benzaldehyde in the Sample
solution (mg/mL)

C7H6O 106.12 Acceptance criteria: 98.0%–102.0%

Benzoic aldehyde;
Phenyl formaldehyde CAS RN®: 100-52-7. IMPURITIES
• LIMIT OF HYDROCYANIC ACID
DEFINITION Sample solution: Shake 0.5 mL of Benzaldehyde with 5 mL
Benzaldehyde contains NLT 98.0% and NMT 102.0% of of water, add 0.5 mL of 1 N sodium hydroxide and 0.1 mL
benzaldehyde (C7H6O). of ferrous sulfate TS, and warm the mixture gently.
Acceptance criteria: Upon the addition of a slight excess of
IDENTIFICATION hydrochloric acid, no greenish-blue color or blue
Change to read: precipitate is produced within 15 min.
• LIMIT OF NITROBENZENE
• A. ▲SPECTROSCOPIC IDENTIFICATION TESTS á197ñ, Infrared Sample solution: Dissolve 1 mL of Benzaldehyde in 20 mL
Spectroscopy: 197F▲ (CN 1-May-2020) of alcohol, and mix with 10 mL of water.
Analysis: Add 1-g portions of zinc and 1-mL portions of 2 N
ASSAY sulfuric acid, as needed, to maintain a brisk evolution of
• PROCEDURE hydrogen for 1 h. Filter, evaporate the liquid to 20 mL, and

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Solution A: Acetonitrile and glacial acetic acid (1000:1, boil 10 mL of the concentrated liquid with 1 drop of
v/v) potassium dichromate TS.
Solution B: Glacial acetic acid and water (1:1000, v/v) Acceptance criteria: No purplish color is produced.
Mobile phase: See Table 1. • CHLORINATED COMPOUNDS
ci Analysis: Wind a strip of 20-mesh copper gauze 1.5 cm wide
Table 1 and 5 cm long around the end of a copper wire. Heat the
Time Solution A Solution B gauze in the nonluminous flame of a Bunsen burner until it
(min) (%) (%) glows without coloring the flame green. Permit the gauze
0 18 82 to cool, and heat several times until a thick coat of oxide
has formed. With a medicine dropper, apply 2 drops of
20 60 40 Benzaldehyde to the cooled gauze, ignite, and permit it to
ffi
30 60 40 burn freely in the air. Again cool the gauze, add 2 more
drops of Benzaldehyde, and burn as before. Repeat this
process until a total of 6 drops have been added and
System suitability solution: 0.1 mg/mL of USP Benzoic ignited. Then hold the gauze in the outer edge of the
Acid RS and 0.06 mg/mL of USP Methylparaben RS in Bunsen flame, adjusted to a height of 4 cm.
acetonitrile
O

Acceptance criteria: Not even a transient green color is

Standard solution: 0.15 mg/mL of USP Benzaldehyde RS in imparted to the flame.
acetonitrile • LIMIT OF ETHYLBENZENE, CYCLOHEXYLMETHANOL, BENZYL
Sample solution: 0.15 mg/mL of Benzaldehyde in ALCOHOL, AND BENZOIC ACID
acetonitrile Sample solution: Neat Benzaldehyde
Chromatographic system Standard solution: 0.1% of USP Ethylbenzene RS, 0.1% of
(See Chromatography á621ñ, System Suitability.) USP Cyclohexylmethanol RS, 0.2% of USP Benzoic Acid RS,
Mode: LC and 0.2% of USP Benzaldehyde RS in USP Benzyl Alcohol RS
Detector: UV 235 nm Chromatographic system
Column: 4.6-mm × 25-cm; 5-µm packing L1 (See Chromatography á621ñ, System Suitability.)
Flow rate: 1.2 mL/min Mode: GC
Injection volume: 10 µL Detector: Flame ionization
System suitability Column: 0.32-mm × 30-m fused silica capillary, coated
Samples: System suitability solution and Standard solution with a 0.5-µm layer of phase G16
Suitability requirements Temperatures
Resolution: NLT 2.0 between benzoic acid and Detector: 310°
methylparaben, System suitability solution Injection port: 200°
Tailing factor: NMT 2.0 for benzoic acid and Column: See Table 2.
methylparaben, System suitability solution
Relative standard deviation: NMT 2.0% for Table 2
benzaldehyde, Standard solution
Hold Time at Fi-
Analysis Initial Temperature Final nal
Samples: Standard solution and Sample solution Temperature Ramp Temperature Temperature
Calculate the percentage of benzaldehyde (C7H6O) in the (°) (°/min) (°) (min)
portion of Benzaldehyde taken: 50 5 220 35

Result = (rU/rS) × (CS/CU) × 100

Carrier gas: Helium
rU = peak response of benzaldehyde from the Sample Flow rate: 1.2 mL/min
solution Injection volume: 0.1 µL
Injection type: Splitless injection

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Printed on: Fri Jan 05 2024, [Link] PM(EST) Status: Currently Official on 06-Jan-2024 DocId: GUID-C59E1D6A-1A19-46B9-921B-2E62997EE426_4_en-US
Printed by: USP NF Official Date: Official as of 01-May-2020 Document Type: NF @2024 USPC
Do Not Distribute DOI Ref: l2i5j DOI: [Link]
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System suitability Result = (rU/rT) × 100

Sample: Standard solution
[NOTE—For relative retention times, see Table 3.] rU = peak response of each impurity from the Sample
solution
Table 3 rT = sum of all the peak responses from the Sample
Relative solution
Retention
Component Time Acceptance criteria
Ethylbenzene 0.45
Each individual impurity: NMT 1.0%
Total impurities: NMT 2.0%
Benzaldehyde 1.00
SPECIFIC TESTS
Cyclohexylmethanol 1.03 • WATER DETERMINATION, Method I á921ñ: NMT 1.5%
Benzyl alcohol 1.45 ADDITIONAL REQUIREMENTS
Benzoic acid 2.04 • PACKAGING AND STORAGE: Preserve in well-filled, tight,
light-resistant containers. Store at room temperature, and
System suitability requirements avoid exposure to excessive heat.
Resolution: NLT 3.0 between benzaldehyde and • USP REFERENCE STANDARDS á11ñ
cyclohexylmethanol USP Benzaldehyde RS
Analysis USP Benzoic Acid RS
USP Benzyl Alcohol RS
Samples: Standard solution and Sample solution
USP Cyclohexylmethanol RS
Calculate the percentage of each impurity in the portion of

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USP Ethylbenzene RS
Benzaldehyde taken:
USP Methylparaben RS

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