-
USP32
附录
1
91
一般鉴别试验:
Under
this heading are placed tests that are frequently
referred to in the Pharmacopeia for the
identification of official articles.
[NOTE
—
The tests are not
intended to be applicable to mixtures of
substances unless so specified.]
此处列举的检查项目都是频繁应用于药典鉴别项下的内容:(注:除另有规定外,不适用于混合物)<
/p>
Acetate
—
When
acetic acid or an acetate is warmed with sulfuric
acid and alcohol, ethyl acetate,
recognizable by its characteristic
odor, is evolved. With neutral solutions of
acetates, ferric chloride TS
produces a
deep red color that is destroyed by the addition
of mineral acids.
醋酸盐:
1
、当醋酸或者醋酸盐与硫酸、乙醇和乙酸乙酯一起加热时,应逐渐产生醋酸的特征气味。< p>
2
、醋
酸盐的中性溶液中加入三氯化铁试液,溶液
应显深红色,加入无机酸后颜色应被破坏。
Aluminum
—
With 6
N ammonium hydroxide, solutions of aluminum salts
yield a gelatinous, white
precipitate
that is insoluble in an excess of 6 N ammonium
hydroxide. 1 N sodium hydroxide or sodium
sulfide TS produces the same
precipitate, which dissolves in an excess of
either of these reagents.
铝:
1
、铝盐溶液中加入
6N
的氨水,应产
生白色胶状沉淀,溶液不能溶解于过量的
6N
的氨水中。
2
、铝
盐溶液加入
1
N
的氢氧化钠或硫化钠试液,应产生白色胶状沉淀,当上述试液过量时,沉淀应溶解。<
/p>
Ammonium
—
Ammonium salts are decomposed by the addition of
an excess of 1 N sodium hydroxide,
with
the evolution of ammonia, recognizable by its odor
and by its alkaline effect upon moistened red
litmus paper exposed to the vapor.
Warming the solution accelerates the
decomposition.
铵:铵盐溶液加入过量的
1N
的氢氧化钠溶液,铵盐应分解发出刺激的氨臭,并使湿润的红色石蕊试纸变
蓝,该反应加热可加速铵盐的分解。
Antimony
—
With
hydrogen sulfide, solutions of antimony (III)
compounds, strongly acidified with
hydrochloric acid, yield an orange
precipitate of antimony sulfide that is insoluble
in 6 N ammonium
hydroxide, but is
soluble in
ammonium sulfide
TS
.
锑:三价锑溶液加入硫化氢盐酸溶液,应产生橘红色硫
化锑沉淀,沉淀不溶于
6N
的氨水,可溶于硫化铵
试液。
Barium
—
Solutions
of barium salts yield a white precipitate with 2 N
sulfuric acid. This precipitate is
insoluble in hydrochloric acid and in
nitric acid. Barium salts impart a yellowish-green
color to a
nonluminous flame that
appears blue when viewed through green glass.
钡:
1
、钡盐溶液与
2
N
的硫酸反应,应产生白色溶液。沉淀不溶于盐酸和硝酸。
2<
/p>
、钡盐于无光焰中发出
淡黄绿光,透过绿色玻璃观察应为蓝色。<
/p>
Benzoate
—
In
neutral solutions, benzoates yield a salmon-
colored precipitate with
ferric
chloride TS
. In
moderately
concentrated solutions, benzoates yield a
precipitate of benzoic acid upon acidification
with 2
N sulfuric acid. This
precipitate is readily soluble in ethyl ether.
苯甲酸盐:
1
、苯甲酸盐的中性溶液与三氯化
铁试液反应应产生橘红色沉淀。
2
、苯甲酸盐的浓溶液被
2N
的硫酸酸化后应产生苯甲酸沉淀,沉淀易溶于乙醚。
Bicarbonate
—
See
Carbonate
.
碳酸氢盐:参照碳酸盐
Bismuth
—
When
dissolved in a slight excess of nitric acid or
hydrochloric acid, bismuth salts yield a white
precipitate upon dilution with water.
This precipitate is colored brown by hydrogen
sulfide, and the
resulting compound
dissolves in a warm mixture of equal parts of
nitric acid and water.
铋:铋盐的水稀释液加入稍过量的硝
酸或者盐酸,应产生白色沉淀。沉淀加入硫化氢后变为棕色,产物溶
于温热的硝酸溶液(
硝酸:水
=1:1
)。
Bisulfite
—
See
Sulfite
.
亚硫酸氢盐:参照硫酸盐。
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Borate
—
To 1 mL
of a borate solution, acidified with hydrochloric
acid to litmus, add 3 or 4 drops of
iodine
TS
and 3
or 4 drops of polyvinyl alcohol solution (1 in
50): an intense blue color is produced. When a
borate is treated with sulfuric acid,
methanol is added, and the mixture is ignited, it
burns with a
green-bordered flame.
硼酸盐:
1
、
1ml<
/p>
硼酸盐溶液用盐酸酸化至对石蕊试纸显酸性,加入
3-4
滴碘试液和
3-4
滴聚乙烯醇溶液
(
1:50
),溶液应显深蓝色。
< br>2
、硼酸盐溶于硫酸,加入甲醇后点燃,火焰边缘应为绿色。
Bromide
—
Solutions of bromides, upon the addition of
chlorine TS, dropwise, liberate bromine, which is
dissolved by shaking with chloroform,
coloring the chloroform red to reddish brown.
Silver nitrate TS
produces in solutions
of bromides a
yellowish
–
white precipitate
that is insoluble in nitric acid and is
slightly soluble in 6 N ammonium
hydroxide.
溴化物:
1
、
溴化物溶液逐滴加入氯试液,游离出溴,用氯仿萃取,氯仿层应为红棕色。
2
、溴化物溶液中
加入硝酸银试液,应产生浅黄色沉淀,沉淀不溶于硝酸,易
溶于
6N
的氨水。
Calcium
—
Solutions of calcium salts form insoluble oxalates
when treated as follows. To a solution of the
calcium salt (1 in 20) add 2 drops of
methyl red TS
, and
neutralize with 6 N ammonium hydroxide. Add 3
N hydrochloric acid, dropwise, until
the solution is acid to the indicator. Upon the
addition of
ammonium
oxalate
TS
, a white precipitate is formed. This
precipitate is insoluble in 6 N acetic acid but
dissolves in
hydrochloric acid. Calcium
salts moistened with hydrochloric acid impart a
transient yellowish-red color to
a
nonluminous flame.
钙:
1
、钙盐溶液(
1:20
)中加入
2
滴甲基红试液,用
6N
的氨水中
和,缓缓滴加
3N
的盐酸使其恰成酸性,
加入草酸铵试液,应生成白色沉淀。沉淀不溶于
6N
乙酸,溶
于盐酸。
2
、用盐酸润湿的钙盐于无光焰中应
< br>呈砖红色。
Carbonate
—
Carbonates and bicarbonates effervesce with acids,
evolving a colorless gas that, when
passed into
calcium
hydroxide TS
, produces a white
precipitate immediately. A cold solution (1 in 20)
of a
soluble carbonate is colored red
by phenolphthalein TS, while a similar solution of
a bicarbonate remains
unchanged or is
only slightly colored.
碳酸盐:
1
、碳酸盐与碳酸氢盐遇酸,剧烈反应,生成的气体通入氢氧化钙溶液中,产生白色沉淀。
2
、碳
酸盐溶液加入酚酞试液显红色,
同浓度的碳酸氢盐也呈现红色或略浅的红色。
Chlorate
—
Solutions of chlorates yield no precipitate with
silver nitrate TS
. The
addition of sulfurous acid
to this
mixture produces a white precipitate that is
insoluble in nitric acid, but is soluble in 6 N
ammonium
hydroxide. Upon ignition,
chlorates yield chlorides, recognizable by
appropriate tests. When sulfuric acid
is added to a dry chlorate,
decrepitation occurs, and a greenish yellow-gas is
evolved.
[
Caution
—
Use
only a small amount of chlorate for
this test, and exercise extreme caution in
performing it.
]
氯酸盐:
1
、氯酸盐溶液加入硝酸银试液不会出现沉淀,当加入亚硫酸盐混合后,产生白
色沉淀,沉淀不溶
于硝酸,可溶于
6N
的氨水。
2
、用适当的方法可证明氯酸盐经点燃或加热应产省氯
气。
3
、向干燥的氯酸
盐上滴加硫酸,
剧烈反应,并产生黄绿色气体。(警告:进行此试验应使用极小量氯酸盐,且操作时要谨
慎小心。)
Chloride
—
With
silver nitrate TS
, solutions
of chlorides yield a white, curdy precipitate that
is insoluble in
nitric acid but is
soluble in a slight excess of 6 N ammonium
hydroxide. When testing amine (including
alkaloidal) hydrochlorides that do not
respond to the above test, add one drop of diluted
nitric acid and
0.5 mL of
silver nitrate TS
to a
solution of the substance being examined
containing, unless otherwise
directed
in the monograph, about 2 mg of chloride ion in 2
mL: a white, curdy precipitate is formed.
Centrifuge the mixture without delay,
and decant the supernatant layer. Wash the
precipitate with three
1-mL portions of
nitric acid solution (1 in 100), and discard the
washings. Add
ammonia TS
dropwise to
this precipitate. It
dissolves readily. When a monograph specifies that
an article responds to the test for
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dry chlorides, mix the solid to be
tested with an equal weight of manganese dioxide,
moisten with sulfuric
acid, and gently
heat the mixture: chlorine, which is recognizable
by the production of a blue color with
moistened starch iodide paper, is
evolved.
氯化物:
1
、加入
硝酸银试液,可产生白色凝乳状沉淀,沉淀不溶于硝酸,但可溶于
6N
< br>的氢氧化铵。
2
、
如果测试胺类
盐酸盐(包括生物碱类)不能如上述反应,除另有规定外,准备供试品溶液
2ml
(约含
2mg
氯离子),加入一滴稀硝酸和<
/p>
0.5ml
硝酸银试液,应出现白色凝乳状沉淀,立即离心分离,
弃去上清液,
沉淀分
3
次用
1ml
硝酸溶液(
1<
/p>
→
100
)洗涤,弃去洗涤液。逐滴滴加
氨试液,沉淀即溶解。
3
、如标准中
规
定只能用干燥固体氯化物实验,将供试品与二氧化锰等量混合,用硫酸润湿,缓缓加热,应产生氯气,
使湿润的淀粉碘化钾试纸变蓝。
Citrate
—
To 15 mL
of pyridine add a few mg of a citrate salt,
dissolved or suspended in 1 mL of water,
and shake. To this mixture add 5 mL of
acetic anhydride, and shake: a light red color is
produced.
柠檬酸盐:取数
mg
柠檬酸盐溶于
1ml
水中,加入
1
5ml
吡啶,振摇使悬浮,再加入
5ml
醋酐,振摇,溶
液应显淡红色。
Cobalt
—
Solutions
of cobalt salts (1 in 20) in 3 N hydrochloric acid
yield a red precipitate when heated on
a steam bath with an equal volume of a
hot, freshly prepared solution of
1-nitroso-2-naphthol (1 in 10) in
9 N
acetic acid. Solutions of cobalt salts, when
saturated with potassium chloride and treated with
potassium nitrite and acetic acid,
yield a yellow precipitate.
钴:
1
、钴盐的
3N
盐酸溶液(
1:20
)与等量的新配的热的
1-
硝基
2-
萘酚的
9N<
/p>
的醋酸溶液(
1:10
)混合,
于蒸气浴中,应产生红色沉淀。
2
、钴盐溶液用
氯化钾饱和,经亚硝酸钾和醋酸处理,应产生黄色沉淀。
Copper
—
Solutions
of cupric compounds, acidified with hydrochloric
acid, deposit a red film of metallic
copper upon a bright, untarnished
surface of metallic iron. An excess of 6 N
ammonium hydroxide, added
to a solution
of a cupric salt, produces first a bluish
precipitate and then a deep blue-colored solution.
With
potassium ferrocyanide
TS
, solutions of cupric salts yield a
reddish-brown precipitate, insoluble in
diluted acids.
铜:
1
、供试品溶液经盐酸酸化后,放入表面光滑明亮的金属铁,在铁表层应形成一层红色的
膜。
2
、铜盐
溶液中加入过量的
6N
的氨水,先产生淡蓝色(青黄色)沉淀,沉淀逐渐变为深蓝色。<
/p>
3
、供试品与亚铁氰
化钾试液反应生成红
褐色沉淀,沉淀不溶于稀酸。
Hypophosphite
—
When strongly heated, hypophosphites evolve
spontaneously flammable phosphine.
Hypophosphites in solution yield a
white precipitate with
mercuric
chloride TS
. This precipitate becomes
gray when an excess of hypophosphite is
present. Solutions of hypophosphites, acidified
with sulfuric
acid, and warmed with
cupric sulfate TS
yield a
red precipitate.
次磷酸盐:
1
、次磷酸盐加强热,产生磷化氢,并能自燃。
2
、
供试品溶液中加入氯化汞试液,产生白色沉
淀,当供试品过量时,沉淀颜色变为灰色。<
/p>
3
、供试品溶液用硫酸酸化后,加入硫酸铜试液,温热,产生红<
/p>
色沉淀。
Iodide
—
Solutions
of iodides, upon the addition of chlorine TS,
dropwise, liberate iodine, which colors the
solution yellow to red. When the
solution is shaken with chloroform, the latter is
colored violet. The iodine
thus
liberated gives a blue color with
starch TS
. Silver nitrate TS
produces, in solutions of iodides, a
yellow, curdy precipitate that is
insoluble in nitric acid and in 6 N ammonium
hydroxide.
碘化物:
1
、
碘化物溶液中逐滴滴加氯试液,碘析出,溶液颜色从黄色变为红色,添加氯仿振摇提取,氯仿
层显紫色。
2
、如上述,析出的含碘溶液加入淀粉试液,溶
液显蓝色。
3
、碘化物溶液中加入硝酸银试液,
应生成黄色凝乳状沉淀,沉淀不溶于硝酸和
6N
的氨水
。
Iron
—
Ferrous and
ferric compounds in solution yield a black
precipitate with
ammonium sulfide
TS
. This
precipitate is
dissolved by cold 3 N hydrochloric acid with the
evolution of hydrogen sulfide.
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