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Tiamina, IP
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Thiamine hydrochloride is a vitamin B1 supplem…

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Available FormatsPharmaceutical substances: Thiamini hydrochloridum

Monographs:
- Thiamine hydrochloride
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formula. C H ClN OS,HCl
12 17 4

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Relative molecular mass. 337.3

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Chemical name. Thiamine chloride, hydrochloride; 3-[(4-amino-2-methyl-5-
pyrimidinyl)methyl]-5-(2-hydroxyethyl)-4-methylthiazolium chloride, mono-hydrochloride; CAS
Reg. No. 67-03-8.

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Requirements

Definition. Thiamine hydrochloride contains not less than 98.0% and not more than 101.0% of
C12H17ClN4OS,HCl, calculated with reference to the dried substance.

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Assay. Dissolve about 0.25 g, accurately weighed, in 30 ml of glacial acetic acid R1, add 10 ml
of mercuric acetate/acetic acid TS, and titrate with perchloric acid (0.1 mol/l) VS as described
under 2.6 Non-aqueous titration, Method A. Each ml of perchloric acid (0.1 mol/l) VS is
equivalent to 16.86 mg of C12H17ClN4OS,HCl.

Mercuric acetate/acetic acid TS.

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Procedure. Dissolve 50 g of mercuric acetate R in sufficient glacial acetic acid R1, that has been
neutralized, if necessary, to crystal violet/acetic acid TS with perchloric acid (0.1 mol/l) VS, to
produce 1000 ml.

Acetic acid, glacial, R.

C2H4O2 (SRIP, 1963, p. 25); d ~ 1.048.

Acetic acid, glacial, R1.

Glacial acetic acid R, that complies with the following tests:

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dichromate. To 10 ml add 1.0 ml of potassium dichromate (0.0167 mol/l)
VS and cautiously add 10 ml of sulfuric acid (~1760 g/l) TS. Cool the solution to room
temperature and allow to stand for 30 minutes. While swirling the solution, dilute slowly and
cautiously with 50 ml of water, cool, and add 1.5 ml of freshly prepared potassium iodide (80
g/l) TS. Titrate the liberated iodine with sodium thiosulfate (0.1 mol/l) VS, adding 3 ml of starch
TS as the end-point is approached. Perform a blank titration and make any necessary
corrections. Not less than 0.60 ml of sodium thiosulfate (0.1 mol/l) VS is consumed.

Substances reducing permanganate. Add 40 ml to 10 ml of water. Cool to 15°C, add 0.30 ml of

potassium permanganate (0.02 mol/l) VS, and allow to stand at 15°C for 10 minutes; the pink
colour is not entirely discharged.

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Crystal violet R.

C25H30ClN3 (SRIP, 1963, p. 73).

Crystal violet/acetic acid TS.

A solution of crystal violet R dissolved in glacial acetic acid R1 containing about 5 g/l.

Methods of Analysis: 2. Chemical methods: 2.6 Non-aqueous

titration

Acids and bases have long been defined as substances that, when dissolved in water, furnish
hydrogen and hydroxyl ions, respectively. This definition, introduced by Arrhenius, fails to
recognize the fact that properties characteristic of acids or bases may also be developed in other
solvents. A more generalized definition is that of Brönsted, who defined an acid as a proton
donor, and a base as a proton acceptor. Even broader is the definition of Lewis, who defined an
acid as any material that will accept an electron pair, a base as any material that will donate an
electron pair, and neutralization as the formation of a coordination bond between an acid and a
base.

The apparent strength of an acid or base is determined by the extent of its reaction with a
solvent. In aqueous solution all strong acids appear equally strong because they react with the
solvent to undergo almost complete conversion to hydronium ion (H3O+) and the acid anion. In a
weakly protophilic solvent such as acetic acid, the extent of formation of the acetonium ion
(CH3COOH2+) due to the addition of a proton provides a more sensitive differentiation of the
strength of acids and shows that the order of decreasing strength for acids is perchloric,
hydrobromic, sulfuric, hydrochloric, and nitric.

Acetic acid reacts incompletely with water to form hydronium ion and is, therefore, a weak acid.
In contrast, it dissolves in a base such as ethylenediamine, and reacts so completely with the
solvent that it behaves as a strong acid.

This so-called levelling effect is observed also for bases. In sulfuric acid almost all bases appear
to be of the same strength. As the acid properties of the solvent decrease in the series sulfuric
acid, acetic acid, phenol, water, pyridine and butylamine, bases dissolved in them become
progressively weaker and the differences between bases are accentuated. In order of decreasing
strength, strong bases of value for non-aqueous titrations are potassium methoxide, sodium
methoxide, lithium methoxide, and tetrabutylammonium hydroxide.

Many water-insoluble compounds acquire enhanced acidic or basic properties when dissolved in
organic solvents. Thus the choice of the appropriate solvent permits the determination of a
variety of such materials by non-aqueous titration. Further, depending upon which part of a
compound is physiologically active, it is often possible to titrate that part by proper selection of
solvent and titrant. Pure compounds can be titrated directly, but it is often necessary to isolate
the active ingredient in pharmaceutical preparations from interfering excipients and carriers.

The types of compounds that may be titrated as acids include acid halides, acid anhydrides,
carboxylic acids, amino acids, enols such as barbiturates and xanthines, imides, phenols,
pyrroles, and sulfonamides. The types of compounds that may be titrated as bases include
amines, nitrogen-containing heterocyclic compounds, quarternary ammonium compounds, alkali
salts of organic acids, alkali salts of inorganic acids, and some salts of amines. Many salts of
halogen acids may be titrated in acetic acid or acetic anhydride after the addition of mercuric
acetate, which removes halide ion as the unionized mercuric halide complex. In the case of
hydrochlorides of weak bases not containing acetylatable groupings it is also possible to titrate in
acetic anhydride without the addition of mercuric acetate and using an indicator such as
malachite green or crystal violet. Titrations carried out in the presence of an excess of acetic

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anhydride must be applied cautiously, however, since any reaction of the anhydride with the
substance being titrated may give rise to low results.

In the titration of a basic compound, a volumetric solution of perchloric acid in glacial acetic acid
is usually used, although perchloric acid in dioxan may be useful in special cases. In the titration
of an acidic compound, a volumetric solution of lithium methoxide in a methanol-toluene solvent
is often used. For many applications it is convenient to use a solution of tetrabutylammonium
hydroxide in toluene; sodium methoxide, formerly in wide use, may often give ri se to
troublesome gelatinous precipitates.

Because of interference by carbon dioxide, solvents for acidic compounds must be protected
from excessive exposure to the atmosphere by a suitable cover or by an inert atmosphere during
the titration. A blank determination should be carried out and the volume generally should not
exceed 0.01 ml of a 0.1 mol/l titrant for each ml of solvent.

The end-point may be determined visually by colour change, or potentiometrically. If the calomel
reference electrode is used, it is advantageous to replace the aqueous potassium chloride
solution in the salt bridge with lithium perchlorate/acetic acid TS for titrations in acidic solvents,
or potassium chloride in methanol for titrations in basic solvents. It should be recognized that
certain indicators in common use (crystal violet, for example) undergo a series of colour changes
and, in establishing a non-aqueous titration method for a particular use, care should be taken to
ensure that the colour change specified as the end-point of the titration corresponds to the
maximum value of dE/dV (where E is the electromotive force and V the volume of titrant) in a
potentiometric titration of the substance under consideration.

When using titrants prepared with solvents that may have a relatively high coefficient of
expansion, for example, glacial acetic acid, toluene, etc., care should be taken to compensate for
differences in temperature that may exist between the time the titrant is used and that at which
it was standardized.

Recommended procedure

Method A (for bases and their salts)

Prepare a solution as specified in the monograph or dissolve the substance being examined in a
suitable volume of glacial acetic acid R1, previously neutralized to crystal violet/acetic acid TS,
warming and cooling if necessary. Alternatively the titration blank for the solvent and indicator
may be established in a separate determination. When the substance is a salt of a hydrohalic
acid, add 10 ml of mercuric acetate/acetic acid TS. When the end-point is determined visually by
colour change, add 2-3 drops of crystal violet/acetic acid TS, and titrate with perchloric acid of
the specified concentration (mol/l) to the appropriate colour change of the indicator. When a
different indicator is specified in the monograph, this indicator should also be used for the
neutralization of the glacial acetic acid R1, and mercuric acetate/acetic acid TS, and the
standardization of the titrant.

When the equivalence point is determined potentiometrically, the indicator is omitted and
neutralization of the solution and standardization of the titrant are also carried out
potentiometrically. A glass electrode and a saturated calomel cell (containing potassium chloride
(350 g/l) TS) as reference electrode, are used. The junction between the calomel electrode and
the titration liquid should have a reasonably low electrical resistance and there should be a
minimum of transfer of liquid from one side to the other. Serious instability may result unless
the connections between the potentiometer and the electrode system are in accordance with the
manufacturer's instructions.

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When the temperature (t2) at which the titration is carried out differs from the temperature (t1)
at which the titrant was standardized, multiply the volume of the titrant required by [1 +
0.001(t1 - t2)] and calculate the result of the assay from the corrected volume.

Monographs: Pharmaceutical substances: Thiamini mononitras -

Thiamine mononitrate

Molecular formula. C12H17N5O4S

Relative molecular mass. 327.4

Graphic formula.

Chemical name. Thiamine nitrate (salt); 3-[(4-amino-2-methyl-5-pyrimidinyl)methyl]-5-(2-

hydroxyethyl)-4-methylthiazolium nitrate (salt); CAS Reg. No. 532-43-4.

Requirements

Definition. Thiamine mononitrate contains not less than 98.0% and not more than 101.0% of
C12H17N5O4S, calculated with reference to the dried substance.

Assay. Dissolve about 0.1 g, accurately weighed, in 30 ml of glacial acetic acid R1, add 0.15 ml
of l-naphtholbenzein/acetic acid TS, and titrate with perchloric acid (0.1 mol/l) VS to a green
end-point, as described under 2.6 Non-aqueous titration, Method A. Each ml of perchloric acid
(0.1 mol/l) VS is equivalent to 16.37 mg of C12H17N5O4S.

1-Naphtholbenzein R.

C27H20O3.

Description. A reddish-brown powder.

Solubility. Practically insoluble in water; soluble in ethanol (~750 g/l) TS, benzene R, ether R,
and glacial acetic acid R.

1-Naphtholbenzein/acetic acid TS.

Procedure. Dissolve 0.2 g of 1-naphtholbenzein R in sufficient glacial acetic acid R to produce

100 ml.

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