The value of hydrochloric acid in the reference book of medicines. Hydrochloric acid hydrochloric acid
6.2. Target Familiarization of students with the properties and methodology for assessing the quality of hydrochloric acid.
Abstracts of the lecture
Hydrochloric acid
Acid hydrochloricum
Hydrochloric acid diluted
Acidum hydrochloricum dilutum
HCl M.m. 36.46
Receipt:
Hydrochloric acid is obtained by dissolving hydrogen chloride in water. The main way industrial production Hydrogen chloride is currently synthesized from hydrogen and chlorine formed during the electrolysis of a sodium chloride solution
Description:
pharmacopoeial preparations of hydrochloric acid are a colorless transparent liquid, sometimes with a yellowish tint, due to the admixture of iron (III) chloride, which can get from the material of the apparatus where the acid is obtained. Hydrochloric acid is miscible with water and alcohol in any ratio, has an acid reaction to litmus.
Diluted hydrochloric acid has the composition: 1 part HCl; 2 parts H2O
Authenticity:
for anion Cl - :
a) with a solution of silver nitrate, a precipitate of silver chloride, soluble in ammonia solution, precipitates
HCl + AgNO 3 \u003d HNO 3 + AgCI
AgCl + NH4OH = Cl + H 2 O
b) when heated with manganese dioxide, free chlorine is released, which is detected by smell
MnO 2 + 4HCl \u003d MnCl 2 + Cl 2 + 2H 2 O
Purity:
To establish the good quality of hydrochloric acid, tests are carried out for possible impurities:
1. Ferric salts (FeCl 3) detect:
a) with a solution of potassium thiocyanate to form red-colored iron thiocyanate (III)
FeCl 3 + 3KSCN Fe(SCN) 3 + 3KCl
Red staining
b) with a solution of potassium hexacyano-ferrate (II) (potassium ferrocyanide) to form "Prussian Blue" of blue color
4FeCl 3 + 3K 4 Fe 4 3 + 12HCl
Prussian blue (blue precipitate)
2. Free chlorine is detected by the action of potassium iodide in the presence of chloroform, which is stained in purple from released iodine
Cl 2 + 2KI I 2 + 2KCl
3. The presence of sulfurous acid, SO 4 2-, As, heavy Me is not allowed.
Quantitation:
1) neutralization method - titration with an alkali solution in methyl orange
With % HCl = 24.8-25.2%; With % HCl razv. =8.2-8.4%
HCl + NaOH NaCl + HOH
2) in terms of density - a certain concentration of acid corresponds to a certain density value (ρ = 1.122-1.124)
Application:
Diluted hydrochloric acid is used in medicine. It is used orally in drops or as a mixture (usually together with pepsin) with insufficient acidity of gastric juice. Often it is prescribed in conjunction with iron preparations, as it helps to improve their absorption.
Storage:
Hydrochloric acid intended for medical purposes should be stored in vials with ground stoppers at room temperature. Acid must not be stored in very warm rooms, as in this case gas (HCl) may be released, which will break the closure of the bottle.
The drug belongs to list B
WFD - 2 ml (40 cap.)
VSD - 6 ml (120 cap.)
If HCl is prescribed in the prescription without indicating the concentration, HCl is dispensed. If HCl is prescribed in a different concentration without indicating that development should be used. HCl, then when calculating HCl razv. accept as 100%
6.4. Illustrative material slides with chemicals and physical properties of hydrochloric acid.
Literature
Main literature:
1. Arzamastsev A.P. Pharmaceutical Chemistry: tutorial, 3rd ed., rev. - M.: GEOTAR-Media, 2008. - 640 p.
2. Belikov V.G. Pharmaceutical Chemistry: Study Guide, 2nd ed. - M.: MEDpress-inform, 2008. - 616 p.
3. Guide to laboratory exercises on pharmaceutical chemistry: E.N. Aksenova, O.P. Andrianova, A.P. Arzamastsev and others - M .: Medicine, 2001. - 384 p.
4. State Pharmacopoeia of the Republic of Kazakhstan: first edition. - 1 volume. - Astana: Ed. house "Zhibek Zholy", 2008. - 592 p.
Additional literature:
1. Analysis of medicinal mixtures / Ed. A.P. Arzamastseva, V.M. Pechennikova, G.M. Rodionova and others - M .: Company Sputnik +, 2000. - 275 p.
2. Arystanova T.A., Ordabaeva S.K. Standardization medicines: tutorial. - Almaty, 2002. - 98 p.
3. State register of medicines. – M.: 2001. – 1277 p.
4. Beisenbekov A.S., Shansharov G.B., Galymov E.G., Beisenbekov N.A. Standardization of drugs: a study guide. - Almaty, 2008. - 167 p.
5. State Pharmacopoeia of the USSR: X edition. – M.: Medicine, 1968. – 1079 p.
6. State Pharmacopoeia of the USSR: XI edition. - M.: Medicine, 1987. - T.1. – 334 p.
7. From substance to drug: textbook / Ed. corresponding member NAS of Ukraine V.P. Chernykh. - Kharkiv: publishing house of NUPh "Golden Pages", 2005. - 1244 p.
1. What chemical reactions the authenticity of hydrochloric acid preparations is established.
2. What methods are used to quantify hydrochloric acid
3. What tests, apart from pharmacopoeial tests, can be used to identify cations and anions that make up the molecules of drugs in this group?
Hydrochloric acid.
Colorless transparent volatile liquid of a peculiar smell, sour taste. Miscible with water and alcohol in all respects, forming acidic solutions. Specific gravity 1.125-1.127.
Store according to list B, in bottles with ground stoppers.
Distinguish:
Hydrochloric acid containing 25% hydrogen chloride - Acid hydrochloricum;
Strong hydrochloric acid (reactive), containing 35-37% hydrogen chloride, Acid hydrochloricum concentratum;
Diluted hydrochloric acid - Acidum hydrochloricum dilutum(transparent colorless liquid miscible with water in all proportions). Obtained by mixing one part hydrochloric acid with two parts water. Contains 8.2-8.4% hydrogen chloride.
For medicinal purposes, dilute hydrochloric acid is used and prescribed in recipes.
Hydrochloric acid converts pepsinogen to active pepsin and provides an acidic environment for its action. In the stomach, it promotes the digestion of proteins, creates conditions for the evacuation of contents into the intestines, regulates the tone of the pyloric sphincter, enhances the secretion of the pancreas and bile, acts antimicrobially, prevents the development of putrefactive and enzymatic processes and prevents the penetration of pathogenic bacteria into the intestines.
It has a pronounced bactericidal effect. As the temperature of the solvent increases, the disinfecting power increases. Destroys spore and vegetative forms of microbes. In the presence of small amounts of sodium chloride, the bactericidal power of the acid increases, since it increases the permeability of the acid into the thickness of the skin, and in large amounts its activity decreases; 2% hydrochloric acid in the presence of 10% sodium chloride destroys anthrax spores in raw hides at 40°C for nine hours.
Inside, it is used for low acidity of gastric juice, enzymatic and putrefactive processes in the stomach, for alkali poisoning, indigestion with symptoms of dyspepsia. Including it is prescribed for chronic hypo- and anacid gastritis, chronic gastroenteritis, tympania, hypotension and atony of the scar, dyspepsia; to accelerate the absorption of iron from the intestines.
In chronic gastritis, the stomach is washed with a 0.3% acid solution. With inflammation of the goiter in birds and cholera in chickens, a 0.4% solution is drunk ad libitum. Artificial gastric juice or 1% hydrochloric acid solution of pepsin (1 l of purified water, 5.0 ml of pure hydrochloric acid and 10.0 g of pepsin) is used for dyspepsia of young animals (calves 100.0 ml, piglets 50.0 ml, lambs 30.0 ml 2-3 times a day).
Hydrochloric acid is used for disinfection of drinking water, hides, unfavorable for anthrax. For disinfection of raw hides, a 2.5% solution based on hydrogen chloride is used with the addition of 10% sodium chloride at a temperature of 40 ° and an exposure of 9 hours. Taking into account the absorption of hydrochloric acid by the skins, an excess amount of acid is taken, but not more than 5% of the weight of the skins. The disinfectant solution is used 10 times the weight of the hide. Based on this, for 100 kg of raw hides, you need to take 1000.0 liters of a 2% solution of hydrochloric acid (20.0 liters of acid) and add 5 liters of acid for adsorption by the skins (you will get a 2.5% pickel solution). Hydrochloric acid (10% solution) with sodium thiosulfate (60% solution), according to the Demyanovich method, is used to treat scabies.
Inside, hydrochloric acid is given in the form of a 0.1-0.4% aqueous solution, preferably with pepsin.
1.2679; G crnt 51.4°C, p crit 8.258 MPa, d crit 0.42 g/cm 3 ; -92.31 kJ / , D H pl 1.9924 kJ / (-114.22 ° C), D H test 16.1421 kJ / (-8.05 ° C); 186.79 J / (mol K); (Pa): 133.32 10 -6 (-200.7 ° C), 2.775 10 3 (-130.15 ° C), 10.0 10 4 (-85.1 ° C), 74, 0 10 4 (-40 ° C), 24.95 10 5 (O ° C), 76.9 10 5 (50 ° C); temperature dependence equation lgp (kPa) = -905.53 / T + 1.75lgT- -500.77 10 -5 T + 3.78229 (160-260 K); coefficient 0.00787; g 23 mN/cm (-155°C); r 0.29 10 7 Ohm m (-85°C), 0.59 10 7 (-114.22°C). See also table. one.
R-value of HC1 at 25 °C and 0.1 MPa (mol.%): in pentane-0.47, hexane-1.12, heptane-1.47, octane-1.63. The p-value of HC1 in alkyl and aryl halides is low, for example. 0.07 / for C 4 H 9 C1. P-value in the range from -20 to 60 ° C decreases in the series dichloroethane-tri-chloroethane-tetrachloroethane-trichlorethylene. R-value at 10°C in a series is approximately 1 / , in carboxylic esters 0.6 / , in carboxylic esters 0.2 / . In stable R 2 O · НCl are formed. The p-value of HC1 is subject to and is for KCl 2.51 10 -4 (800 ° C), 1.75 10 -4 / (900 ° C), for NaCl 1.90 10 -4 / (900 ° FROM).
Salt to-ta. HCl in water is highly exothermic. process, for infinitely razb. water solution D H 0 Hcl -69.9 kJ / , Cl -- 167.080 kJ/; HC1 is fully ionized. The solubility of HC1 in depends on the t-ry (Table 2) and the partial HC1 in the gas mixture. Density of salt dec. and h at 20 °C are presented in Table. 3 and 4. With an increase in t-ry h hydrochloric decreases, for example: for 23.05% hydrochloric at 25 ° C h 1364 mPa s, at 35 ° C 1.170 mPa s. hydrochloric containing h per 1 HC1, is [kJ/(kg K)]: 3.136 (n = 10), 3.580 (n = 20), 3.902 (n = 50), 4.036 (n = 100), 4.061 (n = 200).
HCl forms c (Table 5). In the HCl-water system, there are three eutectic. points: - 74.7 ° C (23.0% by mass of HCl); -73.0°C (26.5% HCl); -87.5°C (24.8% HC1, metastable phase). HCl nH 2 O are known, where n = 8.6 (mp. -40 ° С), 4. 3 (mp. -24.4 ° С), 2 (mp. -17.7 °С) and 1 (mp. -15.35°С). crystallizes from 10% hydrochloric acid at -20, from 15% hydrochloric acid at -30, from 20% hydrochloric acid at -60 and from 24% hydrochloric acid at -80°C. The p-value of halides decreases with increasing HCl in hydrochloric acid, which is used for them.
Chemical properties. Pure dry HCl begins to dissociate above 1500°C, it is chemically passive. Mn. , C, S, P not interact. even with liquid HCl. C, reacts above 650 ° C, with Si, Ge and B-in are present. AlCl 3, with transition metals - at 300 ° C and above. O 2 and HNO 3 are oxidized to Cl 2, with SO 3 gives C1SO 3 H. O p-tions with org. connections see .
FROM hydrochloric acid is chemically very active. Dissolves with the release of H 2 all having negative. ,with me. and forms, allocates free. to-you from such as, etc.
Receipt. In the industry, Hcl get a trace. ways-sulfate, synthetic. and from off-gases (by-products) of a number of processes. The first two methods lose their meaning. So, in the USA in 1965 the share of off-gas salt was 77.6% in the total volume of production, and in 1982-94%.
The production of hydrochloric (reactive, obtained by the sulphate method, synthetic, off-gas) consists in obtaining HCl with the last. his . Depending on the method of heat removal (reaches 72.8 kJ/), the processes are divided into isothermal, adiabatic. and combined.
The sulfate method is based on the interaction. NaCl with conc. H 2 SO 4 at 500-550 ° C. reaction contain from 50-65% HCl (muffle) to 5% HCl (reactor with). It is proposed to replace H 2 SO 4 with a mixture of SO 2 and O 2 (process temperature approx. 540 ° C, cat.-Fe 2 O 3).
The direct synthesis of HCl is based on the chain p-tion: H 2 + Cl 2 2HCl + 184.7 kJ K p is calculated according to the equation: lgK p \u003d 9554 / T- 0.5331g T + 2.42.
R-tion is initiated by light, moisture, solid porous (, porous Pt) and some miners. in-you ( , ). Synthesis is carried out with an excess of H 2 (5-10%) in combustion chambers made of steel, refractory bricks. Naib. modern HCl pollution prevention material - graphite impregnated with phenol-formald. resins. To prevent an explosive nature, they are mixed directly in the flame of the burner. To the top. the zone of the combustion chambers is installed to cool the reaction. up to 150-160°С. The power of modern graphite reaches 65 tons / day (in terms of 35% hydrochloric acid). In case of H 2 deficiency, decomp. process modifications; for example, a mixture of Cl 2 with water is passed through a layer of porous incandescent:
2Cl 2 + 2H 2 O + C: 4HCl + CO 2 + 288.9 kJ
The temperature of the process (1000-1600 ° C) depends on the type and presence of impurities in it, which are (eg, Fe 2 O 3). It is promising to use a mixture of CO with:
CO + H 2 O + Cl 2: 2HCl + CO 2
More than 90% of hydrochloric acid in developed countries is obtained from off-gas HCl, which is formed during and dehydrochlorination of org. compounds, chlororg. waste, obtaining potassium non-chlorinated. etc. Abgazes contain decomp. quantity of HC1, inert impurities (N 2, H 2, CH 4), slightly soluble in org. in-va (, ), water-soluble in-va (acetic acid,), acidic impurities (Cl 2, HF, O 2) and. The use of isothermal it is expedient at a low content of HC1 in exhaust gases (but with the content of inert impurities less than 40%). Naib. promising film, allowing you to extract from the original exhaust gas from 65 to 85% HCl.
Naib. adiabatic schemes are widely used. . Abgases are introduced into the lower. part, and (or dilute hydrochloric) - countercurrent to the top. Salt is heated to t-ry due to the heat of HCl. The change in t-ry and Hcl is given in fig. 1. T-ra is determined by the temperature of the corresponding one (max. t-ra-t. boiling of the azeotropic mixture is approx. 110 ° C).
On fig. 2 shows a typical adiabatic scheme. HCl from off-gases generated during (eg, production). Hcl is absorbed in 1, and the remains of sparingly soluble in org. in-in is separated from after in apparatus 2, further cleaned in tail column 4 and separators 3, 5 and commercial hydrochloric acid is obtained.
Rice. 1. Distribution scheme t-r (curve 1) and
HYDROCHLORIC ACID (hydrochloric acid) - a strong monobasic acid, a solution of hydrogen chloride HCl in water, is one of the most important components of gastric juice; in medicine it is used as a medicine for insufficiency of the secretory function of the stomach. S. to. is one of the most commonly used chem. reagents used in biochemical, sanitary-hygienic and clinical diagnostic laboratories. In dentistry, 10% S. solution is used to whiten teeth with fluorosis (see Teeth Whitening). S. to. is used to obtain alcohol, glucose, sugar, organic dyes, chlorides, gelatin and glue, in the farm. industry, in tanning and dyeing leather, saponification of fats, in the production of activated carbon, dyeing of fabrics, etching and soldering of metals, in hydrometallurgical processes for cleaning boreholes from deposits of carbonates, oxides and other sediments, in electroforming, etc.
S. to. for people in contact with it during the production process, it represents a significant occupational hazard.
S. to. was known as early as the 15th century. Her discovery is attributed to him. Alchemist Valentine. For a long time it was believed that S. to. is an oxygen compound of a hypothetical chemical. element muria (hence one of its names - acidum muriaticum). Chem. The structure of S. to. was finally established only in the first half of the 19th century. Davy (N. Davy) and J. Gay-Lussac.
In nature, free S. practically does not occur, however, its salts sodium chloride (see Table salt), potassium chloride (see), magnesium chloride (see), calcium chloride (see), etc. are very widespread.
Hydrogen chloride HCl under normal conditions is colorless gas with a specific pungent odor; when released into moist air, it strongly "smokes", forming the smallest droplets of aerosol S. to. Hydrogen chloride is toxic. Weight (mass) of 1 liter of gas at 0° and 760 mm Hg. Art. equal to 1.6391 g, air density 1.268. Liquid hydrogen chloride boils at -84.8° (760 mmHg) and solidifies at -114.2°. In water, hydrogen chloride dissolves well with the release of heat and the formation of S. to .; its solubility in water (g/100 g H2O): 82.3 (0°), 72.1 (20°), 67.3 (30°), 63.3 (40°), 59.6 (50° ), 56.1 (60°).
Page to. represents colorless transparent liquid with a sharp smell of hydrogen chloride; impurities of iron, chlorine, or other substances stain S. to. in a yellowish-greenish color.
Approximate value of S.'s concentration to. in percent can be found if beats. S.'s weight to. reduce by one and multiply the resulting number by 200; e.g., if weight S. to. 1.1341, then its concentration is 26.8%, i.e. (1.1341 - 1) 200.
S. to. chemically very active. It dissolves with the release of hydrogen all metals that have a negative normal potential (see Physical and chemical potentials), converts many metal oxides and hydroxides into chlorides, and releases free acids from salts such as phosphates, silicates, borates, etc.
In a mixture with nitric acid (3:1), the so-called. aqua regia, S. to. reacts with gold, platinum and other chemically inert metals, forming complex ions (AuC14, PtCl6, etc.). Under the influence of oxidizers S. to. is oxidized to chlorine (see).
S. to. reacts with many organic matter, for example, proteins, carbohydrates, etc. Some aromatic amines, natural and synthetic alkaloids, and other basic organic compounds form salts with S. to. Paper, cotton, linen, and many artificial fibers are destroyed by S. to.
The main method for producing hydrogen chloride is synthesis from chlorine and hydrogen. The synthesis of hydrogen chloride proceeds in accordance with the reaction H2 + 2C1-^2HCl + 44.126 kcal. Other methods for producing hydrogen chloride are chlorination of organic compounds, dehydrochlorination of organic chlorine derivatives, and hydrolysis of certain inorganic compounds with the release of hydrogen chloride. Less often, in the lab. practice, they use the old method of producing hydrogen chloride by the interaction of common salt with sulfuric acid.
A characteristic reaction to S. to. and its salts is the formation of a white cheesy precipitate of silver chloride AgCl, soluble in excess aqueous ammonia:
HCl + AgN03 - AgCl + HN03; AgCl + 2NH4OH - [Ag (NHs)2] Cl + + 2H20.
Store S. to. in glassware with ground stoppers in a cool room.
In 1897, IP Pavlov found that the parietal cells of the gastric glands of humans and other mammals secrete S. to a constant concentration. It is assumed that the mechanism of S.'s secretion to. consists in the transfer of H+ ions by a specific carrier to the outer surface of the apical membrane of the intracellular tubules of parietal cells and in their entry after additional conversion into gastric juice (see). C1~ ions from the blood penetrate into the parietal cell while simultaneously transferring the bicarbonate ion HCO2 in the opposite direction. Due to this, C1 ~ ions enter the parietal cell against the concentration gradient and from it into the gastric juice. The parietal cells secrete a solution
Page to., concentration to-rogo makes apprx. 160 mmol!l.
Bibliography: Volfkovich S. I., Egorov A. P. and Epshtein D. A. General chemical technology, vol. 1, p. 491 and others, M.-L., 1952; Harmful substances in industry, ed. N. V. Lazarev and I. D. Gadaskina, vol. 3, p. 41, L., 1977; Nekrasov B.V. Fundamentals of General Chemistry, vol. 1 - 2, M., 1973; Emergency care for acute poisoning, Handbook of toxicology, ed. S. N. Golikova, p. 197, M., 1977; Fundamentals of forensic medicine, ed. N. V. Popova, p. 380, M.-L., 1938; Radbil O. S. Pharmacological bases for the treatment of diseases of the digestive system, p. 232, M., 1976; Rem and G. Course of inorganic chemistry, trans. from German, vol. 1, p. 844, M., 1963; Guidelines for forensic medical examination of poisonings, ed. R. V. Berezhny and others, p. 63, M., 1980.
N. G. Budkovskaya; N. V. Korobov (farm.), A. F. Rubtsov (court.).
HC1 M.v. 36.46
Description. Colorless transparent volatile liquid, peculiar smell, sour taste.
Solubility. Miscible with water and alcohol in all proportions, forming strongly acidic solutions.
Authenticity. A solution of the drug 1: 10 gives a characteristic reaction to chlorides. When the preparation is heated with manganese dioxide, chlorine is released.
Density. 1.122 – 1.124
sulfate ash. From 10 ml. drug should not exceed 0.01%
quantitation. 10 ml is poured into a small conical flask with a ground stopper. of water and weigh accurately, then add 3 ml. of the preparation, mix well, stopper and weigh accurately again. The contents of the flask are titrated with 1N sodium hydroxide solution until the color changes from pink to orange-yellow. The indicator is methyl orange.
Storage. List B, in flasks with ground stoppers.
Aqua pro injectionibus
Water for injections
Description: colorless, transparent liquid, odorless and tasteless. pH 5.0 to 7.0. Dry residue no more than 0.001%. Water should not contain chlorides, sulfates, calcium and heavy metal ions, reducing agents, nitrates, nitrites, carbon dioxide. Ammonia content is allowed no more than 0.00002%.
Water for injection should be pyrogen-free and free of antimicrobial substances and other additives. Application: use freshly prepared water for injection or store under certain conditions.
Storage: stored at a temperature of 5 ° to 10 ° C or from 80 ° to 95 ° C in closed containers made of materials that do not change the properties of water, protecting water from mechanical impurities. Store no more than 24 hours.
On the labels of containers for collecting and storing water for injection, there must be a sign that the contents are not sterilized (FS 42-2620-97).
7. Statement of the technological process
Auxiliary work (BP 1)
7.1.1 Receipt of ampoules (BP 1.1)
Dart making. Dart is made from liquid glass mass in ATG 8-50 lines. The length of the tubes is 1500±50 mm, the cut is made mechanically and thermally.
Dart calibration
Tube diameter - from 8.00 to 27.00 mm. Calibration is carried out according to the outer diameter in two sections at a distance of 350 mm from the middle of the tube on the machine N.A. Philippines. Five calibers, 2 of each size, are fixed on the vertical frame of the machine at a distance of 700 mm between them, the slots of which increase from bottom to top by 0.25 mm. With the help of grippers, the tubes are fed stepwise from below to the first calibers, if dimensions allow, the tube passes through them and rolls into the accumulator. If the tube diameter is larger than the gap, the tube rises to the next higher clearance gauges.
Productivity - 30 kg of tubes per hour. Washing and drying
Produced in a chamber-type tube washer and dryer.
250-350 kg of tubes are loaded into the container in a vertical position, and it is rolled into the chamber using a pneumatic drive.
The doors of the chamber are sealed and the system of automatic control of the washing mode is switched on. The chamber with tubes is filled with tap water, the liquid is heated to a boil. Soaking is continued for 1 hour at 60°C. Then bubbling is carried out by supplying steam for 40 minutes. After that, the liquid from the chamber is drained. Demineralized water is supplied under pressure to the shower device. With the help of pneumatic cylinders, the nozzles of the showering device are moved in a horizontal plane, showering is carried out for 30-60 minutes. The liquid from the chamber is drained.
Drying is carried out with hot filtered air at a temperature
60°C - 15-20 minutes.
The quality of washing is checked visually by examining the inner surface while illuminating the bundle of tubes from the opposite side. The surface must be smooth without noticeable mechanical inclusions.
Dressing of ampoules
Ampoules are made on rotary glass-forming machines IO-8. They have a pinch, the nominal volume of ampoules is 1 ml.
The tubes are loaded into storage drums designed for each of the 16 pairs of upper and lower cartridges and pass through 6 positions:
tubes are fed from the storage drum into the cartridge. With the help of the limit stop, their length is set. The top cartridge compresses the tube, leaving it at a constant height in all positions;
burners with a wide flame fit the rotating tube and heat them until the glass softens. At the same time, the lower cartridge, moving along the copier, rises up and clamps the lower part of the tube;
the lower cartridge, continuing to move along the copier, descends down to the softened glass of the tube protrudes into the capillary;
a burner with a sharp flame approaches the top of the capillary. At this position, a segment of the capillary occurs;
simultaneously with the cutting off of the capillary, the bottom of the next ampoule is sealed;
the lower cartridge releases the clamps and the resulting ampoule is lowered onto the inclined tray. The tube with a sealed bottom approaches the limit stop of the 1st position and the cycle of operation of the machine is repeated. At the moment of release of the clamps of the lower cartridge, under the action of gravity of the ampoule, a very thin capillary is pulled out at the tapping point, which breaks off when the ampoule falls and rotates simultaneously. Due to this, the tightness of the ampoules is broken, and they are obtained without vacuum.
The optimum flame temperature of the burners is 1250-1350°C.
Preparation of containers, ampoules, vials, closures (BP 1.2)
Ampoule annealing
Annealing is carried out in electric quenching furnaces. Ampoules are placed in trays capillaries up and served on the loading table. With the help of a chain conveyor, they move through the tunnel, passing in turn the heating, holding and cooling chambers. In the heating chamber, the ampoules are quickly heated to a temperature of 600°C and enter the holding chamber, which is held for 7-10 minutes at the same temperature. During this time, residual stresses in the glass are relieved, organic pollutants are burned, and glass dust is fused into the walls of the ampoule. Then the trays with ampoules enter the cooling chamber with filtered air. In the first zone of this chamber, there is a slow, gradual cooling with heated air at a temperature of about 200 ° C for 30 minutes. Such conditions ensure uniform cooling of the outer and inner walls of the ampoules. In the second zone of the chamber, the ampoules are air-cooled to 60°C in 5 minutes and the tray approaches the unloading table.
The quality of annealing is checked by the polarization-optical method - the difference in the path of the rays is measured on a polariscope - a PKS-250 polarimeter according to GOST 732E.74. Residual voltage is not allowed, creating a specific difference in the path of the rays of more than 8 m
Opening of capillaries
The operation is carried out so that the ampoules are of the same height. The ends of the capillaries at the site of opening should have even and smooth edges.
The opening of ampoules is carried out on semi-automatic rotary machines. A rotor with nests for ampoules is used as a conveyor; they move to a rotating disk knife. Near the knife, the ampoule begins to rotate due to its friction against a fixed plate mounted on the body. The disk knife makes a circular incision on the capillary, at the site of which an opening occurs due to thermal shock when heated by a burner. After opening the capillary
melted by a burner, and the ampoule enters the hopper for collection in cassettes
External washing of ampoules
Cassettes with ampoules are placed in a bath on a stand and showered with demineralized water at a temperature of 60°C. During washing, the cassette with ampoules performs a rotational movement under the pressure of water jets, which contributes to the same cleaning of the entire outer surface.
Ampoule internal washing
It is carried out in a vapor-condensation way, automatically. The cassette with ampoules, capillaries down, is placed in the working container, the lid is closed, and the device is purged with steam through the refrigerator and the working container for 6 seconds. Air is forced out of the apparatus and its walls are heated. The sprayer is fed cold water with a temperature of 8-10°C under a pressure of 147038.75 Pa. As a result of the contact of steam with droplets of cold water from the sprayer in the refrigerator and the working container, a vacuum is created. To remove air from the ampoules, the vacuum is repeated. The working container is filled with demineralized water at a temperature of 80-90°C through a pipeline to a predetermined level, which ensures complete immersion of the ampoule capillaries in water. Steam is supplied to the apparatus through the refrigerator for 4 seconds, and then cold water is supplied to the atomizer. The vacuum created in this case is extinguished by steam under pressure. Under the action of hydraulic shock associated with a sharp pressure drop, water in the form of a turbulent flow rushes into the ampoule. When a vacuum occurs, the water boils violently. To remove water from the ampoules, a vacuum is created by steam condensation. In the same portion of washing water, up to 9 water hammers can occur. From the working tank, water with impurities is removed through the valve by supplying steam under pressure. After that, water is displaced from the ampoules by creating a vacuum. A new portion of water is poured into the working container (80-90 ° C); the cycles are repeated until the ampoules are completely cleaned. In the last cycle, rinsing with purified water with four water hammers is carried out. Then a vacuum is created in the apparatus without supplying water to the working container. Water is finally removed from the ampoules, they are dried.
7 .1.3 Obtaining and preparing the solvent (BP 1.3)
Getting demineralized water
Demineralization of water is carried out using ion exchange, based on the use of ion exchangers. The cation exchanger in the H-form exchanges all the cations contained in the water, the anion exchanger in the OH-form exchanges all the anions.
As a cation exchanger, a strongly acidic sulfonic cation exchanger KU-2 is used, anion exchanger - a strongly basic AV-171.
The ion-exchange unit consists of 3 pairs of cation and anion columns. Tap water enters the cationite column, passes through a layer of cationite, then anionite, is fed to a filter with a pore size of not more than 5-10 microns (to remove particles of destruction of ion-exchange resins), is heated in a heat exchanger to a temperature of 80-90°C.
Regeneration of ion exchangers
Before regeneration, the ion exchangers are loosened by a reverse flow of tap water. Cationites are regenerated in several steps. 1, 0.7 and 4% solutions of sulfuric acid. Before draining into the sewer, the acid from the column is neutralized with marble chips. Anion exchangers are restored in 3 doses: 2.6, 1.6 and 0.8% sodium hydroxide solution.
After treatment with solutions of reagents, the columns are washed with water to a predetermined pH value.
Obtaining water for injection
Water for injection preparations is obtained by distillation of demineralized water in a three-vessel water distiller "Finn-aqua". II, I buildings, heats up and enters the evaporation zone, which contains a system of tubes heated from the inside by heating steam. The heated water is directed to the outer surface of the heated tubes in the form of a film with the help of a distributor, flows down them and is heated to a boil.
An intensive steam flow is created in the evaporator, with special guides it is given a spiral rotational movement from the bottom up at a high speed - 20-60 m / s, the centrifugal force that occurs in this case presses the drops against the walls, and they flow into the lower part of the housing. The purified secondary steam is directed to the preheating chamber and heater tubes of the II housing. The casing is heated by technical steam, which enters the preheating chamber, then into the evaporator tubes and is discharged through the steam locking device into the technical condensate line. The excess feed water is fed through a tube from the bottom of I and II buildings to the evaporators, where water also flows down in the form of a film along the outer surface (heated inside the tubes) through the pipe into the condenser-refrigerator as the target distillate. In housing III, feed water comes from the lower part of housing II. Condensation inside the pipes III housing is also transferred through the pipe to the condenser-refrigerator. Heating of the preheating zone and tubular evaporators of buildings II and III is carried out by the secondary steam of buildings I and II. The secondary purified steam from the II building through the pipe enters directly into the refrigerator and condenses. The combined condensate from the refrigerator passes through a special heat exchanger, where it maintains a temperature of 80 to 95°C. At the exit from it, the electrical conductivity slows down in the distillate. If the water is of insufficient quality according to this indicator, it is discarded into the sewer.
The resulting water enters the system for collection and storage. The system consists of two tanks with a steam jacket and a sterilizing air filter to a pump that pumps water from one tank to another at a constant speed of 1-3 m/s.
The temperature of the circulating water is maintained by heat exchangers. The connecting pipes must have a slope of 2-3°. The maximum shelf life of water for injection is 24 hours (under aseptic conditions).
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