Methylene Chloride

Methylene Chloride USP NF Grade
Dichloromethane USP NF Grade
CH2Cl2 84.93
Methane, dichloro-.
Dichloromethane --- [CAS 75-09-2].
Methylene Chloride contains not less than 99.0 percent of CH2Cl2.
[Caution: Perform all steps involving evaporation of methylene chloride in a well-ventilated fume hood. ]
Packaging and storage: Preserve in tight containers.

Identification: Place about 5 mL into a glass-stoppered, 10-mL conical flask, and shake for several minutes. Remove the stopper, quickly withdraw a portion of the vapor into a 50-mL syringe that is not fitted with a needle, and inject the vapor into a suitable evacuated gas cell: the IR absorption spectrum of the vapor shows strong doublet peaks at 7.8 5m and 7.9 5m and at 13.2 5m and 13.4 5m, and relatively few minor peaks.
Specific gravity: between 1.318 and 1.322.
Water: not more than 0.02%.
Limit of hydrogen chloride: Into each of 2 glass-stoppered, 50-mL color-comparison cylinders having an internal diameter of 20 mm place 10 mL of water, 2 drops of phenolphthalein, and sufficient 0.010 N sodium hydroxide to produce a pink color that persists after vigorous shaking for 30 seconds, and is of equal intensity in each cylinder. [NOTE: In the following steps, take special care to avoid contamination with carbon dioxide.] Into one of the cylinders place 20.0 mL of Methylene Chloride and 0.70 mL of 0.010 N sodium hydroxide, and shake again. The pink color in the test cylinder is at least as intense as that in the comparison cylinder, and the color persists for not less than 15 minutes (0.001%).
Limit of nonvolatile residue: Evaporate 50 g in a platinum or porcelain dish on a steam bath, and dry at 105C for 30 minutes: the weight of the residue does not exceed 1 mg (0.002%).
Heavy metals: Evaporate 15 mL (20 g) in a glass evaporating dish on a steam bath to dryness. Cool, add 2 mL of hydrochloric acid, and slowly evaporate again on a steam bath to dryness. Dissolve the residue in 1 mL of 1 N acetic acid, add 24 mL of water, and mix: the limit is 1 ppm.
Free chlorine: To 10 mL add 10 mL of water and 0.1 mL of potassium iodide, shake for 2 minutes, and allow the liquids to separate: the lower layer does not show a violet tint.
Assay: By chromatographic system.

Dichloromethane BP Ph Eur Grade:
Methylene Chloride Ph. Eur.
CH2Cl2 --- 84.9 --- CAS 75-09-2
Action and use: Excipient.

DEFINITION
Dichloromethane.
It may contain maximum 2.0 per cent V/V of anhydrous ethanol and/or maximum 0.03 per cent V/V of 2-methylbut-2-ene as stabiliser.

CHARACTERS
Appearance: Clear, colourless, volatile liquid.
Solubility: Sparingly soluble in water, miscible with ethanol (96 per cent).

IDENTIFICATION
First identification: B, C
Second identification: A, D, E
A. Relative density (see Tests).
B. Refractive index (see Tests).
C. Infrared absorption spectrophotometry
D. Heat 2 mL with 2 g of potassium hydroxide and 20 mL of ethanol (96 per cent) R under a reflux condenser for 30 min. Allow to cool. Add 15 mL of dilute sulfuric acid and filter. To 1 mL of the filtrate add 1 mL of a 15 g/L solution of chromotropic acid, sodium salt, 2 mL of water and 8 mL of sulfuric acid. A violet colour is produced.
E. 2 mL of the filtrate obtained in identification test D gives reaction of chlorides.

TESTS
Appearance: It is clear and colourless.
Acidity: To 50 mL of methanol previously neutralised to 0.1 mL of bromothymol blue solution, add 50 g of the substance to be examined. Not more than 0.15 mL of 0.1 M sodium hydroxide is required to change the colour of the indicator to blue.
Relative density: 1.320 to 1.332.
Refractive index: 1.423 to 1.425.
Ethanol, 2-methylbut-2-ene and volatile impurities: To pass the test.
Impurities percentage contents Limits:
ethanol: maximum 2.0 per cent V/V;
2-methylbut-2-ene: maximum 300 ppm V/V;
impurity A: maximum 10 ppm V/V;
impurity B: maximum 50 ppm V/V;
sum of impurities other than ethanol and 2-methylbut-2-ene: maximum 0.1 per cent V/V;
reporting threshold: 50 ppm V/V; the reporting threshold does not apply to impurity A.
Free chlorine: Place 5 mL in a ground-glass-stoppered tube. Add 5 mL of a 100 g/L solution of potassium iodide and 0.2 g of soluble starch. Shake for 30 s and allow to stand for 5 min. No blue colour develops.
Residue on evaporation: Maximum 20 ppm.
Water: Maximum 0.02 per cent m/m, determined on 10.00 g.

STORAGE
In an airtight container, protected from light.

LABELLING
The label states the name and concentration of any stabilisers.

IMPURITIES
A. carbon tetrachloride
B. trichloromethane (chloroform)
D. methanol.

Methylene Chloride FCC Food Grade
Dichloromethane; Methylene Dichloride
CH2Cl2 --- Formula wt 84.93
CAS: [75-09-2]

DESCRIPTION
Methylene Chloride occurs as a clear, colorless, nonflammable liquid. It is soluble in about 50 parts of water, and is miscible with alcohol, with acetone, with chloroform, and with ether.
Its refractive index at 20C is about 1.424.
Function: Extraction solvent.

REQUIREMENTS
Assay: Not less than 99.0% of CH2Cl2.
Acidity (as HCl): Not more than 10 mg/kg.
Distillation Range: Between 39.0° and 41.0°.
Free Halogens: Passes test.
Lead: Not more than 1 mg/kg.
Nonvolatile Residue: Not more than 0.015%.
Specific Gravity: Between 1.318 and 1.323.
Water: Not more than 0.02%.

Dichloromethane Analytical Reagent Grade:
Methylene Chloride
CH2Cl2 --- Formula Wt 84.93
CAS Number 75-09-2

Suitable for use in high-performance liquid chromatography, extraction-concentration analysis, ultraviolet spectrophotometry, or general use. Product labeling shall designate the one or more of these uses for which suitability is represented on the basis of meeting the relevant requirements and tests. The ultraviolet spectrophotometry and liquid chromatography suitability requirements include all of the requirements for general use. The extraction-concentration suitability requirements include only the general use requirement for color.

REQUIREMENTS
General Use
Appearance: Clear
Assay: 99.5% CH2Cl2.

MAXIMUM ALLOWABLE
Color (APHA): 10
Residue after evaporation: 0.002%
Titrable acid: 0.0003 meq/g
Free halogens: Passes test
Water (H2O): 0.02%.

Certifications :
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