Sealed ampoules

Crotonaldehyde (2-butenal) [123-73-9] M 70.1, b 104-105 , d 0.851, n 1.437. Fractionally distd under N2, through a short Vigreux column. Stored in sealed ampoules. Stabilised with 0.01% of 2,6-di-tert-butyl-p-cresol... 

Pivaloyl chloride (trimethylacetyl chloride) [3282-30-2] M 120.6, b 57.6"/150mm, 70.5-71/250mm, 104"/754mm, 104-105"/atm, 105-108"/atm, d 1.003, n p 1.4142. First check the IR to see if OH hands are present. If absent, or present in small amounts, then redistil under moderate vac. If present in large amounts then treat with oxalyl chloride or thionyl chloride and reflux for 2-3h, evap and distil residue. Strongly LACHRYMATORY - work in a fumecupboard. Store in sealed ampoules under N2. [Traynham and Battiste J Org Chem 22 1551 1957, Grignard reactns Whitmore et al. J Am Chem Soc 63 647 1941.]... 

Thioglycollic acid [68-11-1] M 92.1, b 95-96 /8mm, d 1.326, n 1.505, pK 3.42, pK j 10.20. Mixed with an equal volume of benzene, the benzene is then distd to dehydrate the acid. After heating to 100° to remove most of the benzene, the residue was distd under vacuum and stored in sealed ampoules at 3°. [Eshelman et al. Anal Chem 22 844 I960.]... 

VinyInaphthaIene [826-74-4] M 154.2, b 124-12S /lSnim. Fractionally distd under reduced pressure on a spinning-band column, dried with CaH2 and again distd under vacuum. Stored in sealed ampoules in a freezer. 

N-(Thexyl dimethylsilyl)dimethylamine (N-[2,3-dimethyl-2-butyl]dimethylsilyl dimethyl-amine) [81484-86-8] M 187.4, b 156-160°/720mm. Dissolve in hexane, filter, evaporate and distil. Colourless oil extremely sensitive to humidity. It is best to store small quatities in sealed ampoules after distillation. For estimation of purity crush an ampoule in excess O.IN HCl and titrate the excess acid with O.IM NaOH using methyl red as indicator. [Helv Chim Acta 67 2128 1984.]... 

Vanadyl trichloride (VOCI3) [7727-18-6] M 173.3, m-79.5°, b 124.5-125.5°/744mm, 127.16°/760mm, d 1.854, d 1.811. Should be lemon yellow in colour. If red it may contain VCI4 and CI2. Fractionally distil and then redistil over metallic Na but be careful to leave some residue because the residue can become EXPLOSIVE in the presence of the metal USE A SAFETY SHIELD and avoid contact with moisture. It readily hydrolyses to vanadic acid and HCl. Store in a tightly closed container or in sealed ampoules under N2. [Inorg Synth 1 106 1939, 4 80 1953.]... 

R-(+)-Pantothenic acid sodium salt (7V-[2,4-dihydroxy-3,3-dimethylbutyryl] P-alanine Na salt) [867-81-2] M 241.2, [aJ +27.1 (c 2, H2O), pK 4.4 (for free acid). Crystd from EtOH, very hygroscopic (kept in sealed ampoules). The free acid is a viscous hygroscopic oil with [a] +37.5 (c 5, H2O), easily destroyed by acids and bases. 

In some circumstances it may be considered preferable to prepare the standard solution by making use of one of the concentrated volumetric solutions supplied in sealed ampoules which only require dilution in a graduated flask to produce a standard solution. 

Aliquots of the reaction mixture are placed in an inert atmosphere in sealed ampoules or flasks which are plunged in a thermostated oil bath. At different reaction times one ampoule is opened and its content is titrated. 

The checkers employed a sealed ampoule of bromomethane of b.p 5° (obtained from Eastman Organic Chemicals) which was cooled to 0° and opened. After a boiling chip had been added to the ampoule, it was connected to the gas-inlet tube of the reaction apparatus with rubber tubing, and the ampoule was warmed in a water bath to distil the bromomethane into the reaction vessel. 

Nitsche (242) grew single crystals of Hg3Te2l2 up to 4 x 4 x 4 mm in size by sublimation of the microcrystalline product, containing an excess of Te, in a sealed ampoule at 550°C. Within 10 days, crystals were formed at the colder (530°C) part of the ampoule. 

Batsanov et al. 23) reacted sulfur with PtCU and PtBr2 by heating mixtures of the reactants in evacuated, sealed ampoules. At 100 -200°C after 12-24 h, sulfide chlorides PtCljS (1.70 < x < 2 0.6 s y < 3.35) and sulfide bromides PtBr S (1.87 < x 2.06 0.84 y s 1.80) were formed. The compositions depended on the initial PtX2 S ratio, and the temperature. At 320-350°C, loss of chlorine led to the compounds PtClS (1.7 y 1.9). According to their X-ray powder patterns, all of these products retained the main structural features of the original platinum halides. From considerations of molar volumes, the authors deduced the presence of polysulfide anions. 

The compounds AlYX are best prepared by direct reaction between the respective aluminum halide and chalcogenide in a sealed ampoule at 350°C. The reaction is complete after 2 weeks. In the case of the iodides, a mixture of A1 and I2 (molar ratio 3 10) is used instead of AII3. Other preparative methods, such as the reaction of an aluminum halide with Zn or Cd chalcogenide, or with the chalcogen itself, are applicable to the bromide and chloride only, and give poor yields (15-20%) (158, 159, 266, 327, 328). 

Growth of single crystals. Crystals of the aluminum selenide halides (needles, maximum length 15 mm) were grown by vapor transport in sealed ampoules between two temperatures (380 and 320°C for Al-SeCl, and 350 and 300°C for AlSeBr and AlSel) over a period of two months. A large excess of the halogenide was used (266). 

The chalcogenide bromides and chlorides may be prepared by the reaction of the halide with the respective chalcogenide in a sealed ampoule. A mixture of gallium metal and chalcogen may be used, instead of the chalcogenide. The chalcogenide iodides are S3mthesized directly from the elements. The exact preparative conditions are listed in Table XVIII 160,165). 

Indium chalcogenide chlorides and bromides are obtained by heating mixtures of the chalcogenide and the halide in sealed ampoules to temperatures between 200 and 420°C (see Table XIX). For the preparation of the chalcogenide iodides. In and I2 are used instead of Inlj. InTel may be synthesized directly from the elements (161). 

The sulfide halides TISX are prepared by heating a stoichiometric mixture of the thallium halogenide and sulfur in a sealed ampoule at 180°C for 30 h. The mixture is then slowly cooled to room temperature. The compounds TlSeX are obtained by reaction between thallium metal and selenide halide at 280°C during 40 h (22). On heating TlYCl to 500°C in vacuo, the compounds TI4YCI4 result (322). Dissolution of... 

The determined products do not add to 100 % since insoluble tarry products are also obtained. A similar product mixture is obtained by heating compound 1 in a sealed ampoule to bOO C (ref. 12). These results show that the thermochemistry of 1 depends strongly on whether it is performed with pure compound 1 or if 1 is heated within a polymeric matrix. 

Biological indicators (Bis) for use in thermal, chemical or radiation sterilization processes consist of standardized bacterial spore preparations which are usually in the form either of suspensions in water or culture medium or of spores dried on paper, aluminium or plastic carriers. As with chentical indicators, they are usually placed in dummy packs located at strategic sites in the sterilizer. Alternatively, for gaseous sterihzation these may also be placed within a tubular hehx (Line-Pickerill) device. After the sterilization process, the aqueous suspensions or spores on carriers are aseptically transferred to an appropriate nutrient medium which is then incubated and periodically examined for signs of growth. Spores of Bacillus stearothermophilus in sealed ampoules of cultrrre medium are used for steam sterilization morritoring, and these may be incubated directly at 55°C this eliminates the need for an aseptic transfer. 

Barker and Kahn have made a detailed study of the exchange in carbon tetrachloride media using the isotope " Sb to label the Sb(III) species. The reaction was carried out in sealed ampoules covered with A1 foil in the presence of an atmosphere of He or Ar gas. The separation method used involved complexing the Sb(V) with fluoride (brought about by addition of ethanol, HCl and HF) followed by precipitation of the Sb(III) with H2S and finally addition of boric acid and HCl, removal of the CCI4, and treatment with H2S to remove the Sb(V). Zero-time exchange was 5 %. 

The products formed after heating dried P-carotene at 180°C for 2 hr in a sealed ampoule (SI) with air circulation (S2) stirring with starch and water (S3) and during extrusion process (S4) were isolated. - In all systems, 5,6-epoxy-P-carotene (trans and two cis isomers), 5,8-epoxy-P-carotene (trans and four cis isomers), and 5,6,5,6-diepoxy-P-carotene were identified, along with 5,6,5,8-diepoxy-P-carotene in systems S3 and S4. Later on, along with the epoxides previously found, 5 P-apocarotenals with 20 to 30 carbons, P-caroten-4-one, and 6 different P-carotene cis isomers were isolated in systems S3 and S4, whereas lower numbers of degradation products were found in the other systems. ... 

Adiabatic calorimetry. Dewar tests are carried out at atmospheric and elevated pressure. Sealed ampoules, Dewars with mixing, isothermal calorimeters, etc. can be used. Temperature and pressure are measured as a function of time. From these data rates of temperature and pressure rises as well as the adiabatic temperature ri.se may be determined. If the log p versus UT graph is a straight line, this is likely to be the vapour pressure. If the graph is curved, decomposition reactions should be considered. Typical temperature-time curves obtained from Dewar flask experiments are shown in Fig. 5.4-60. The adiabatic induction time can be evaluated as a function of the initial temperature and as a function of the temperature at which the induction time, tmi, exceeds a specified value. 

The first official injection (morphine) appeared in the British Pharmacopoeia (BP) of 1867. It was not until 1898 when cocaine was added to the BP that sterilization was attempted. In this country, the first official injections may be found in the National Formulary (NF), published in 1926. Monographs were included for seven sterile glass-sealed ampoules. The NF and the United States Pharmacopeia (USP) published chapters on sterilization as early as 1916, but no monographs for ampoules appeared in USP until 1942. The current USP contains monographs for over 500 injectable products [1]. 

Glass-seal ampoules provide the most impervious barrier for gas transmission. A butyl rubber stock is used with rubber-stoppered products that are sensitive to oxygen because it provides better resistance to gas permeation than other rubber stocks. 

Process controls include daily testing of water for injection (USP), conformation of fill doses and yields, checking and approving intermediate production tickets, and checking label identity and count. Finished product control includes all the tests necessary to ensure the potency, purity, and identity of the product. Parenteral products require additional tests, which include those for sterility, pyrogens, clarity, and particulate analysis, and for glass-sealed ampoules, leaker testing. 

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