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EUROPEAN PHARMACOPOEIA 6.0

small and form a terminal spike. They are pentamerous and borne in the axils of hairy bracts, the calyces closely surrounded by numerous terminal hooked spires, which occur on the rim of the hairy receptacle. The petals are free, yellow and deciduous. Fruit-bearing obconical receptacles, with deep furrows and hooked bristles, are usually present at the base of the inflorescence. B. Reduce to a powder (355) (2.9.12). The powder is yellowish-green to grey. Examine under a microscope using chloral hydrate solution R. The powder shows numerous straight of bent, unicellular, long thick-walled (about 500 m) trichomes finely warty and sometimes spiraly marked ; fragments of parenchyma with prisms and cluster crystals of calcium oxalate ; fragments of leaf epidermis with sinuous walls, those of the lower epidermis with abundant stomata, mostly anomocytic but occasionally anisocytic ; ovoid to subspherical-pollen grains, with 3 pores and a smooth exine ; fragments of glandular trichomes with a multicellular uniseriate stalk and a spherical unicellular or quadricellular head ; groups of fibres and spiral and bardered-fitted vessels from the stem.

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AIR, MEDICINAL Aer medicinalis

DEFINITION Compressed ambient air. Content : 20.4 per cent V/V to 21.4 per cent V/V of oxygen (O2). CHARACTERS A colourless, odourless gas. Solubility : at a temperature of 20 C and a pressure of 101 kPa, 1 volume dissolves in about 50 volumes of water.

PRODUCTION Carbon dioxide : maximum 500 ppm V/V, determined using an infrared analyser (2.5.24). Gas to be examined. Use the substance to be examined. It must be filtered to avoid stray light phenomena. C. Thin-layer chromatography (2.2.27). Reference gas (a). Use a mixture of 79 per cent V/V of Test solution. To 2.0 g of the powdered drug (355) nitrogen R1 and 21 per cent V/V of oxygen R containing (2.9.12) add 20 ml of methanol R. Heat with shaking at less than 1 ppm V/V of carbon dioxide R1. 40 C for 10 min. Filter. Reference gas (b). Use a mixture of 79 per cent V/V of Reference solution. Dissolve 1.0 mg of rutin R and nitrogen R1 and 21 per cent V/V of oxygen R containing 1.0 mg of isoquercitroside R in 2 ml of methanol R. 500 ppm V/V of carbon dioxide R1. Plate : TLC silica gel plate R. Calibrate the apparatus and set the sensitivity using Mobile phase : anhydrous formic acid R, water R, ethyl reference gases (a) and (b). Measure the content of carbon dioxide in the gas to be examined. acetate R (10:10:80 V/V/V). Carbon monoxide : maximum 5 ppm V/V, determined using Application : 10 l, as bands. an infrared analyser (2.5.25). Development : over a path of 12 cm. Gas to be examined. Use the substance to be examined. It Drying : at 100-105 C. must be filtered to avoid stray light phenomena. Reference gas (a). Use a mixture of 79 per cent V/V of Detection : spray the still warm plate with a 10 g/l nitrogen R1 and 21 per cent V/V of oxygen R containing solution of diphenylboric acid aminoethyl ester R in methanol R and then with a 50 g/l solution of macrogol less than 1 ppm V/V of carbon monoxide R. 400 R in methanol R. Allow the plate to dry in air for Reference gas (b). Use a mixture of 79 per cent V/V of 30 min. Examine in ultraviolet light at 365 nm nitrogen R1 and 21 per cent V/V of oxygen R containing Results : see below the sequence of the zones present in 5 ppm V/V of carbon monoxide R. the chromatograms obtained with the reference and test Calibrate the apparatus and set the sensitivity using solutions. reference gases (a) and (b). Measure the content of carbon monoxide in the gas to be examined. Top of the plate Sulphur dioxide : maximum 1 ppm V/V, determined using An orange fluorescent zone may an ultraviolet fluorescence analyser (Figure 1238.-1). be present (quercitroside) The apparatus consists of the following : Isoquercitroside : an orange An orange fluorescent zone fluorescent zone (isoquercitroside) a system generating ultraviolet radiation with a An orange fluorescent zone wavelength of 210 nm, made up of an ultraviolet lamp, (hyperoside) a collimator, and a selective filter ; the beam is blocked Rutin : an orange fluorescent An orange fluorescent zone periodically by a chopper rotating at high speeds ; zone (rutin) Reference solution Test solution a reaction chamber, through which flows the gas to be examined ; a system that detects radiation emitted at a wavelength of TESTS 350 nm, made up of a selective filter, a photomultiplier Loss on drying (2.2.32) : maximum 10.0 per cent, determined tube and an amplifier. on 1.000 g of the powdered drug (355) (2.9.12) by drying Gas to be examined. Use the substance to be examined. It in an oven at 105 C for 2 h. must be filtered. Total ash (2.4.16) : maximum 10.0 per cent. Reference gas (a). Use a mixture of 79 per cent V/V of nitrogen R1 and 21 per cent V/V of oxygen R. ASSAY Reference gas (b). Use a mixture of 79 per cent V/V of Carry out the determination of tannins in herbal drugs nitrogen R1 and 21 per cent V/V of oxygen R containing (2.8.14). Use a 1.000 g of powdered drug (180) (2.9.12). 0.5 ppm V/V to 2 ppm V/V of sulphur dioxide R1. 1118 See the information section on general monographs (cover pages)

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Air, medicinal

Figure 1238.-1. UV fluorescence analyser Calibrate the apparatus and set the sensitivity using reference gases (a) and (b). Measure the content of sulphur dioxide in the gas to be examined. Oil : maximum 0.1 mg/m3 calculated for atmospheric pressure and at 0 C, determined using a measuring system such as described in Figure 1238.-2. The apparatus consists of the following : an on-off valve (1), a three-way valve (2), an oil cone (3), a bypass line (4), a pressure-regulator (5), a flow-metering device (6). All of the apparatus is cleaned beforehand, using trichlorotrifluoroethane R free from oil and grease. Place a micro fibre-glass filter in the oil cone (3) ; this filter has the following characteristics : 100 per cent borosilicate glass without binder ; resistant to heat treatment at 500 C (to eliminate organic traces) ; 99.999 per cent retention efficiency for NaCl particles with a diameter of 0.6 m. Close the on-off valve (1) ; the substance to be examined enters the bypass line (4) and purges the three-way valve (2), the pressure-regulator (5) and the flow-metering device (6). Close the inlet valve of the compression and filtration system : open the on-off valve (1) and set the three-way valve (2) to the position allowing passage between the oil cone and the pressure-regulator. Open the inlet valve and set the pressure-regulator (5) so that the flow indicated by the flow-metering device (6) is 20 litres/min. Pass 100.0 litres of the substance to be examined through the system. Test solution. Remove the micro fibre-glass filter and place in an airtight container. Carefully cut up the micro fibre-glass filter and place the pieces in 25.0 ml of trichlorotrifluoroethane R. Reference solutions. Prepare the reference solutions with quantities of oil (used for the lubrication of the compression system) ranging from 0.05 g/ml to 0.5 g/ml in trichlorotrifluoroethane R. Measure the absorbance of the test solution and the reference solutions, using an appropriate infrared spectrophotometer, at 2960.3 cm 1, 2927.7 cm 1 and 2855.0 cm 1. The sum of the 3 absorbances gives the absorbance of the oil. Use potassium bromide cells with a pathlength of several centimetres. Plot the calibration curve from the absorbances obtained with the reference solutions and determine the quantity of oil from this curve. Nitrogen monoxide and nitrogen dioxide : maximum 2 ppm V/V in total, determined using a chemiluminescence analyser (2.5.26). Gas to be examined. Use the substance to be examined. Reference gas (a). Use a mixture of 79 per cent V/V of nitrogen R1 and 21 per cent V/V of oxygen R containing less than 0.05 ppm V/V of nitrogen monoxide and nitrogen dioxide. Reference gas (b). Use a mixture of 2 ppm V/V of nitrogen monoxide R in nitrogen R1. Calibrate the apparatus and set the sensitivity using reference gases (a) and (b). Measure the content of nitrogen monoxide and nitrogen dioxide in the gas to be examined.

Figure 1238.-2. Measuring system for oil General Notices (1) apply to all monographs and other texts 1119

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systems operating at a pressure not greater than 10 bars and Water : maximum 67 ppm V/V, determined using an electrolytic hygrometer (2.5.28), except where the competent a temperature not less than 5 C : maximum 870 ppm V/V, authority decides that the following limit applies to medicinal determined using a water vapour detector tube (2.1.6). air generated on-site and distributed in pipe-line systems operating at a pressure not greater than 10 bars and a temperature not less than 5 C : maximum 870 ppm V/V, determined using an electrolytic hygrometer (2.5.28). Assay. Determine the concentration of oxygen in air using a paramagnetic analyser (2.5.27). IDENTIFICATION First identification : C. Second identification : A, B. A. In a conical flask containing the substance to be examined, place a glowing wood splinter. The splinter remains glowing. B. Use a gas burette (Figure 1238.-3) of 25 ml capacity in the form of a chamber in the middle of which is a tube graduated in 0.2 per cent between 19.0 per cent and 23.0 per cent, and isolated at each end by a tap with a conical barrel. The lower tap is joined to a tube with an olive-shaped nozzle and is used to introduce the gas into the apparatus. A cylindrical funnel above the upper tap is used to introduce the absorbent solution. Wash the burette with water R and dry. Open the 2 taps. Connect the nozzle to the source of the substance to be examined and set the flow rate to 1 litre/min. Flush the burette by passing the substance to be examined through it for 1 min. Close the lower tap of the burette and immediately afterwards the upper tap. Rapidly disconnect the burette from the source of the substance to be examined. Rapidly give a half turn to the upper tap to eliminate any excess pressure in the burette. Keeping the burette vertical, fill the funnel with a freshly prepared mixture of 21 ml of a 560 g/l solution of potassium hydroxide R and 130 ml of a 200 g/l solution of sodium dithionite R. Open the upper tap slowly. The solution absorbs the oxygen and enters the burette. Allow to stand for 10 min without shaking. Read the level of the liquid meniscus on the graduated part of the burette. This figure represents the percentage V/V of oxygen. The value read is 20.4 to 21.4. C. It complies with the limits of the assay. TESTS Carbon dioxide : maximum 500 ppm V/V, determined using a carbon dioxide detector tube (2.1.6). Sulphur dioxide : maximum 1 ppm V/V, determined using a sulphur dioxide detector tube (2.1.6). Oil : maximum 0.1 mg/m , determined using an oil detector tube (2.1.6).
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Figure 1238.-3. Gas burette STORAGE As a gas, in suitable containers complying with the legal regulations or as a gas supplied by a pipe network. IMPURITIES A. carbon dioxide, B. sulphur dioxide, C. nitrogen monoxide, D. nitrogen dioxide,

Nitrogen monoxide and nitrogen dioxide : maximum 2 ppm V/V, determined using a nitrogen monoxide and nitrogen dioxide detector tube (2.1.6). Carbon monoxide : maximum 5 ppm V/V, determined using a carbon monoxide detector tube (2.1.6).

E. oil, Water vapour : maximum 67 ppm V/V, determined using F. carbon monoxide, a water vapour detector tube (2.1.6), except where the competent authority decides that the following limit applies to medicinal air generated on-site and distributed in pipe-line G. water. See the information section on general monographs (cover pages)

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