-
USP32
附录
1
91
一般鉴别试验：
主要的问题是里
面的一些英文
and
是翻译成“和”还是“或”
Under this heading are placed
tests that are frequently referred to in the
Pharmacopeia for
the identification of
official articles. Before using any acid or base
to modify the PH of the
sample
solution, make sure that the added substance will
not interfere with the results of
the
test. [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。
在用任何酸或基础
物质调整样品
溶液的
PH
前，要保证所
加的物质不会影响到检测结果：（注：除另有规定外，不适用于混
合物）
Acetate
—
Dissolve
about 30mg of the substance to be examined in 3ml
of the prescribed
solution. Adjust the
PH of the solution with sodium hydroxide to
slightly alkaline. Add
0.25ml of
lanthanum nitrate TS. If a white precipitate is
formed, filter the solution. Add
successively 0.1ml of iodine and
potassium iodide TS 3 and 0.1ml of ammonia TS 2 to
the
solution. I f no blue color is
observed, heat carefully to boiling. In the
presence of acetates,
a dark color
develops or a blue precipitate is fprmed. With
neureal solutions of acetates,
ferric
chloride TS produces a red color tha is destroyed
by the addition of mineral acids.
醋酸盐：
将
30mg
被检物溶于
3ml
的水中，或用
3ml
的规定溶液。用氢氧化钠调
节
PH
至弱
碱。加入
< br>0.25ml
硝酸镧试液。如出现白色沉淀，过滤溶液。先后加入
0.1ml
的碘和碘化钾
试液
3
和
0.1ml
的氨试液至溶液中。如
没得到蓝色，小心加热至沸腾。如硝酸盐出现深色或
蓝色沉淀物。取醋酸的中性溶液，加
三氯化铁试液出现红色，加无机酸，红色破坏。
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
、加入<
/p>
6N
的氨水，应产生白色胶状沉淀，沉淀物在过量的
6N
的氨水中不溶。
2
、加
入
1N
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。
Ammonium
—
Add
0.2g of magnesium oxide to the solution under
test. Pass a current of
air through the
mixture, and direct the gas that escapes to just
beneath the surface of an
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indicator solution, prepared by mixing
1ml of 0.1M hydrochloric acid and 0.05ml of methyl
red TS2. In the presence of ammonium,
the color of the indicator solution is changed to
yellow. After directing the gas into
the indicator solution for a sufficient period of
time, add
1ml of freshly prepared
sodium cobaltinitrite TS to the indicator
solution. Upon the addition
of the
sodium cobaltinitrite TS, a yellow precipitate is
formed when ammonium is present.
铵：溶液中加
入
0.2g
氧化镁。混合物产生气体，把产生的气体通入指示剂
的液面下，
（指示
剂配制：
1ml0.
1M
盐酸和
0.05ml
的甲基红试液
2.
）指示液变黄色。气体通入指示液充分后，
加入
1ml
新配的亚硝酸钴钠试液。由于亚硝酸钴钠试
液的加入，铵会出现黄色沉淀物。
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：三价锑溶液加盐酸酸化后，通硫化氢，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 2N
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
、加
2N
硫酸，钡盐溶液产生白色沉淀。沉淀在盐酸和硝酸中不溶。
2
、钡盐于无色光
焰中发出淡黄绿光，透过绿色玻璃观察应为蓝色。
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 2N 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产生赭色沉淀。
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，沉淀在乙醚中易溶。
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
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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。
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
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。
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 6N 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，应产生浅黄色絮乳状沉淀，沉淀不溶于硝
酸，微溶于
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
6N ammonium hydroxide.
Add 3N 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 6N
acetic acid but dissolves in hydrochloric acid.
Calcium
salts moistened with
hydrochloric acid impart a transient yellowish-red
color to a
nonluminous flame.
钙：按以下方式钙盐溶液形成不溶的草酸盐。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。用盐酸润湿的钙盐在无色光焰中
应呈砖红色。
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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，产生无色气体，通入氢氧化钙溶液中，立
即产生白色沉淀。
2
、可溶性冷的碳酸盐溶液（
1
→
20
）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 6N 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，当加入亚硫酸后，混合物产生白色
沉淀，沉淀不溶于硝酸，可溶于
6N
的氨水。
2
、用适当的方法表明氯酸盐经点燃应产生氯
化物。<
/p>
3
、在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 6N 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
2mg of chloride
ion in 2mL: 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 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.
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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，但可溶于稍过量
的
6N
氨水。
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
1
滴稀硝酸和
0.5ml
硝酸银试液，应出现
白色凝乳状沉淀，立即离心，弃去上清液，沉淀分
3
次用
1ml
硝酸溶液（
1
→
100
）洗涤，
弃去
洗涤液。逐滴滴加氨试液，沉淀即溶解。
3
、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，
该方法只能用于专论中干燥的
固体氯化物实
验。
Citrate
—
To 15mL
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：
取数毫克柠檬酸盐溶解或悬浮在
1ml
水中，加入
15ml
吡啶，振摇，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
< br>盐酸溶液（
1
→
20
）与等体积新配的热
1-
硝基
2-
萘酚的
9N
的醋酸溶液
（
1
→
10
）混合，在蒸气浴中，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 6N
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
的金属铜膜。
2
、铜盐溶液中加入过
量的
6N
的氨水，先产生淡蓝色（青白色）沉淀，沉淀
逐渐变为深蓝色。
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
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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。
3
、供试品溶液用硫酸酸化后，
加入硫酸铜试液，温热，产生红色沉淀。
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 6N
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，氯仿层显紫色。
2
、如上述，析出的碘加入淀粉
试液，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 3N hydrochloric acid with the
evolution of
hydrogen sulfide.
< br>铁：铁和亚铁化合物的溶液中加入硫化铵试液，产生黑色沉淀，沉淀溶于冷的
3N
的含有硫
化氢的盐酸溶液。
Ferric Salts
—
Acid solutions of ferric salts yield a dark blue
precipitate with
potassium
ferrocyanide TS
. With an
excess of 1 N sodium hydroxide, a reddish-brown
precipitate is
formed. With
ammonium thiocyanate TS
,
solutions of ferric salts produce a deep red color
that is not destroyed by dilute mineral
acids.
铁盐：
1
、铁盐的酸溶
液加入
亚铁氰化钾
溶液，生成深蓝色沉淀，加入过量的
1N
的氢氧化
钠，沉淀变为红褐色。
2
、向铁盐溶液中加入硫氰酸铵试液，溶液即显深红色，加入稀无机
酸，颜色不改变。
Ferrous
Salts
—
Solutions of ferrous
salts yield a dark blue precipitate with
potassium
ferricyanide
TS
. This precipitate is insoluble in 3N
hydrochloric acid but is decomposed by
1N sodium hydroxide. With 1N sodium
hydroxide, solutions of ferrous salts yield a
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