How to judge the true and false of choline chloride?

How to judge the true and false of choline chloride?

Several methods for distinguishing the authenticity of choline chloride choline
is a kind of B-group vitamin (VB4), the common have pure 70% and 75% water
agent, 50% and 60% powder 4 kinds. One of the common powder, but serious
adulteration, quality problems, with the international gb10818-89 (hereinafter
referred to as International) detection, and can not identify the authenticity
of the content can not be measured to reflect the intrinsic quality, especially
the product of choline chloride-trimethylamine residue.

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Chlorinated choline 50% and 60% of the powder is generally white or tawny
(depending on the shape of different and different) dry liquid powder or
particles, with strong hygroscopicity, a special odor. However, the absorption
of carbon dioxide and moisture in the air, can emit ammonia odor, should be
noted.

In order to effectively identify all kinds of adulterated choline chloride, the
following 4 methods can be used:

1 GB no water droplets to be called 80 ℃ dry 3h samples 0.7g in the triangle
bottle, add 40ml methanol, fully shake 30min after filtration, and then
separately with 20ml, 15ml, 15ml methanol washing precipitation 3 times, the
filtrate and lotion combined, evaporation to dry in the water bath, and then
dissolved with 20ml ice acetic acid, 2ml acetic anhydride, 10ml acetic acid
mercury and raindrop crystal violet indicator, with perchlorate standard
solution (concentration of 0.1MOL/1) titration to pure blue, while doing blank.

Choline chloride content = (CX (v-v0) x139.63)/mx1000 Note: The molecular
formula of choline chloride is c5h14nclo, the molecular weight is 139.632
nitrogen method 2.1 to the mineral as the carrier of the choline chloride
mineral carrier mainly silica, or to reduce the cost of adding a certain amount
of stone powder, The determination method of silicon-calcium carrier is as
follows: The Kjeldahl nitrogen method is used to determine the nitrogen content
in the sample 0.5g and 0.6g.

Choline chloride content = amount of nitrogen in choline chloride/pure choline
chloride content (10.03) x100%2.2 the commonly used plant material carrier of
choline chloride as the carrier of vegetable is corn cob powder, wheat bran and
rice husk powder, etc., the determination method is: said the sample product 1g
or so in the funnel with the white qualitative filter paper, Rinse 10 times with
water, remove the filter paper drying, the Kjeldahl nitrogen method to determine
the nitrogen content of N1, also called 0.5g ~0.6g Direct determination of
nitrogen content N2.

Choline chloride content = (N2-N1)/10.03×100% type: The nitrogen content
measured by n2–Direct sample; Nitrogen content of n1–residue (carrier),
10.03-pure choline chloride content.

3 Silver method is called 0.5g sample in 250ml iodine volumetric, add 50ml water
shake evenly, add 0.5ml potassium chromate, with silver nitrate standard
solution titration to brick red, at the same time do blank.

① chloride content = (CX (v-v0) x139.63)/Mx1000② chloride ion content = (CX
(v-v0) x35.50)/mx1000-type: 50% the percentage of chloride in choline chloride
is 12.71%;60% The percent content of chlorine ion in choline chloride is
15.25%;c–nitrate standard solution concentration, mol; v–nitrate droplets
Quantitative, ml, v0–blank drops quantitative, ml, 139.63-choline chloride
molar mass, g/mol;35.50-chloride ion molar mass mol.

44-Admittance The sample is about 1g (called to 0.0002g) in the 100M1 capacity
bottle, add water to dissolve and dilute to scale shake, filter, and accurately
measure filtrate 10M1 in 100ml beaker, add 20ml water, l drop aluminum
trichloride (calculated), 20m1 four sodium benzene (2%), Excellent grade pure
four benzene boron sodium 2g, add water dissolve dilute to 100ml, add 2 drops
0.5mol/1 NaOH shake evenly place 24h, filtration, the Solution shelf life 5d),
constantly shake 30min, with the pre-drying weighing 4# crucible filtration,
water

Wash the Beaker 4 times, each time about 10ml, and filtrate together, will
precipitate in 105 ℃ drying 2h, remove into the dryer cooling, weighing.

Choline chloride content = (sedimentation quality (g) x0.3298×100)/sample
quality (g) X10:0.3298–1g precipitation is equivalent to the quality of 0.3298g
choline chloride.

If the true choline chloride, the results of the above 4 methods should be
consistent; If one of the measured values differs greatly from the results of
other methods, there may be adulteration. The suspicious samples were selected
by carbon tetrachloride flotation, and the precipitates were qualitatively
analyzed to determine the adulterated material. Common adulteration:
trimethylamine hydrochloride, ammonium chloride, sodium chloride, potassium
chloride, nitrate, nitrite, urea, urea aldehyde polymers. (There are some
inferior stone powder, the naked eye can see, with 1:1 hydrochloric acid
titration has a large number of bubbles produced.) Carbon tetrachloride
flotation Method: said the sample about 30g in the 250ml liquid funnel, plus
carbon tetrachloride 170ml, full oscillation 10min, after the 30min, the lower
layer of precipitation carefully placed in a dry small beaker, boiling water
bath steam dry. Take a little precipitation, add sodium hydroxide, water bath
heating with ammonia (or trimethylamine, etc.) containing nitrogen, there will
be ammonia volatilization; Otherwise, it may be hydrochloride (sodium chloride,
potassium chloride) and so on. Whether the addition of hydrochloric acid, can
also be used to measure the content of chlorine ions, according to the level of
its content to judge.

At the same time, attention should be paid to: ① in the process of synthesis of
choline chloride, one of the products of trimethylamine hydrochloride residue
increased by 1%, by the determination of the non-aqueous titration, the content
of choline chloride will increase 1.4%, and the true content of choline chloride
more deviation; The content of choline chloride containing nitrate, nitrite,
urea and urea aldehyde ② could not be determined by the method of fixed
nitrogen. The content of choline chloride mixed with hydrochloric acid in ③
could not be determined by the method of silver content. ④ Chemical Industry
standard hg2941-1999 (instead of hg2941-1989).