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HG/T 3696.3-2011 PDF in English


HG/T 3696.3-2011 (HG/T3696.3-2011, HGT 3696.3-2011, HGT3696.3-2011)
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Standards related to: HG/T 3696.3-2011

HG/T 3696.3-2011: PDF in English (HGT 3696.3-2011)

HG/T 3696.3-2011
CHEMICAL INDUSTRY STANDARD OF
THE PEOPLE’S REPUBLIC OF CHINA
ICS 71.060.01;71.060.99
G 10
Filing No.: 34583-2012
Replacing HG/T 3696.3-2002
Inorganic chemicals for industrial use - Preparation of
standard and reagent solutions for chemical analysis - Part
3: Preparations of reagent solutions
ISSUED ON: DECEMBER 20, 2011
IMPLEMENTED ON: JULY 01, 2012
Issued by: Ministry of Industry and Information Technology of PRC
Table of Contents
Foreword ... 3 
1 Scope ... 5 
2 Normative references ... 5 
3 Warning ... 5 
4 General provisions ... 5 
5 Preparation method ... 6 
Index ... 27 
Inorganic chemicals for industrial use - Preparation of
standard and reagent solutions for chemical analysis - Part
3: Preparations of reagent solutions
1 Scope
This standard specifies the preparation of preparations, products, reagents, solutions,
buffer solutions, indicators, indicator solutions, which are commonly used in the
chemical analysis of inorganic chemical products.
This standard applies to the preparation of preparations and products, which are
required for chemical analysis of inorganic chemical products. It can also be used for
chemical analysis of other chemical products.
2 Normative references
The following documents are essential to the application of this document. For the dated
documents, only the versions with the dates indicated are applicable to this document;
for the undated documents, only the latest version (including all the amendments) is
applicable to this standard.
GB/T 6682-2008 Water for analytical laboratory use - Specification and test
methods
GB/T 9733 Chemical reagent - General method for the determination of carbonyl
compounds
3 Warning
Some of the reagents used in the preparation method of this Part of are toxic or
corrosive, so the operator must be careful! If splashed on the skin, rinse
immediately with water. If serious, seek medical attention immediately.
4 General provisions
4.1 The water, which is used in this Part, refers to the grade-3 water, which is specified
in GB/T 6682-2008, unless other requirements are specified.
4.2 The purity of the reagents, which are used in this Part, shall be above analytical
grade.
4.3 If the concentration is expressed in unit mass and volume, the concentration is
expressed in grams per liter (g/L).
4.4 When the solution appears turbid, precipitated, changes in color or exceeds the
specified limit, it shall be prepared again.
4.5 Unless otherwise specified, the solutions in this Part refer to aqueous solutions;
dilution refers to dilution with water.
4.6 Unspecified ethanol, which is used in this Part, is commercially available 95%
ethanol.
5 Preparation method
5.1 Preparation
5.1.1 Carbon dioxide-free water
Pour water into the flask. Boil it for 10 min. Immediately use a rubber stopper, which
is equipped with a soda lime tube, to plug it tightly. Let it stand for cooling. The service
life is one week.
5.1.2 Oxygen-free water
Pour water into the flask. Boil it for 1 h. Immediately use a rubber stopper, which is
equipped with a glass conduit, to plug it tightly. The conduit is connected to a washing
bottle, which contains 100 g/L pyrogallic acid alkaline solution. Cool it down. The
service life is 2 days.
5.1.3 Ammonia-free water
Take 2 parts of strong basic anion exchange resin and 1 part of strong acid cation
exchange resin. Fill them in an exchange column, which has a diameter of 3 cm and a
length of 50 cm, in turn. Pass water through the exchange column, at a flow rate of 3
mL/min ~ 5 mL/min. The service life is one week.
5.1.4 Ammonia-free sodium hydroxide solution
Inject the sodium hydroxide solution of the required concentration into the flask. Boil
if for 30 min. Use a rubber stopper of the safety funnel (ring-neck double-ball), which
contains (1 + 4) sulfuric acid solution (see Figure 1). Cool it. Use an ammonia-free
water to dilute it to original volume.
The sulfur dioxide gas is passed into the water, at normal temperature 15 °C ~ 25 °C,
until saturated. Prepare it before use.
5.1.7 Saturated hydrogen sulfide water
Pass hydrogen sulfide gas into carbon dioxide-free water, until saturated. Prepare it
before use.
5.1.8 Aqua regia
Slowly pour 1 volume of nitric acid into 3 volumes of hydrochloric acid. Mix well.
Prepare it before use.
5.1.9 Methanol without carbonyl groups
Measure 2000 mL of methanol. Pour it into a 3000 mL distillation flask. Add 10.0 g of
2,4-dinitrophenylhydrazine and 0.5 mL of hydrochloric acid. Reflux on a water bath for
2 h. Heat for distillation. Discard the first 50 mL of distillate. Collect the distillate. Store
it in a brown stoppered bottle. The carbonyl-free methanol, which is prepared by the
above method, shall be determined, according to the provisions of GB/T 9733; the
carbonyl content shall not exceed 0.001%.
5.1.10 Aldehyde-free ethanol
Measure 2000 mL of ethanol. Pour it into a 3000 mL distillation flask. Add 10.0 g of
2,4-dinitrophenylhydrazine and 0.5 mL of hydrochloric acid. Reflux on a water bath for
2 hours. Heat to evaporate it. Discard the initial 50 mL of distillate. Collect the distillate.
Store it in a brown stoppered bottle.
Take 5 mL of aldehyde-free ethanol, which is prepared by the above method. Add 5 mL
of water. Cool it to 20 °C. Add 2 mL of magenta-sulfurous acid solution. Leave it for
10 min. There shall be no obvious red color.
5.2 Products
5.2.1 Lead acetate cotton
Take absorbent cotton. Soak it in 50 g/L lead acetate [Pb(CH3COO)2 • 3H2O] solution.
Remove excess solution. Dry it. Store it in an airtight bottle.
5.2.2 Calcium and magnesium-free sodium chloride
Mix 1 volume of the saturated solution of guaranteed pure sodium chloride with 1
volume of dehydrated ethanol. Stir it continuously, until no crystallization appears.
Carry out suction filtration. Dry the crystallization at 105 ° C ~ 110 ° C. Prepare for use.
5.2.3 Starch-potassium iodide test paper
Add 0.20 g of potassium iodide, into 100 mL of newly prepared 10 g/L starch solution.
Put ashless filter paper into the solution and soak it. Then take it out to dry in the dark.
Store tightly closed in a clean, dry brown bottle.
5.2.4 Mercury bromide test paper
Weigh 1.25 g of mercury bromide. Dissolve it in 25 mL of ethanol. Soak the ashless
filter paper in the solution for 1 hour. Take it out to dry in the dark. Store it in a clean
and dry brown bottle.
5.3 Reagents and solutions
5.3.1 Disodium EDTA-Mg solution [c(EDTA-Mg) = 0.01 mol/L]
Take 25 mL of disodium EDTA solution [c(EDTA) ≈ 0.02 mol/L] and 25 mL of
magnesium chloride [c(MgCl2) ≈ 0.02 mol/L]. Mix well. Add 10 mL of ammonia-
ammonium chloride buffer solution A (pH ≈ 10) and a small amount of chrome black T
indicator. Use disodium EDTA solution [c(EDTA) ≈ 0.02 mol/L] or magnesium
chloride [ c(MgCl2) ≈ 0.02 mol/L], to adjust the solution, until it just becomes pure blue
or purple.
5.3.2 Acetic acid solution
5% acetic acid solution (w = 5%): Measure 48 mL of glacial acetic acid. Mix it with
961 mL of water.
30% acetic acid solution (w = 30%): Measure 298 mL of glacial acetic acid. Mix with
731 mL of water.
5.3.3 Glyoxal acetal di-o-aminophenol ethanol solution (2 g/L)
Weigh 0.20 g of glyoxal acetal di-o-aminophenol (calcium reagent). Dissolve it in
ethanol. Use ethanol to dilute it to 100 mL.
5.3.4 Lead acetate (alkali) solution
Weigh 5.0 g of lead acetate [Pb (CH3COO)2 • 3H2O] and 15.0 g of sodium hydroxide.
Dissolve it in 80 mL of water. Dilute it to 100 mL. Store it in polyethylene plastic bottles.
5.3.5 Sodium diethyldithiocarbamate solution (1 g/L)
Weigh 0.10 g of sodium diethyldithiocarbamate (copper reagent). Dissolve it in water.
Dilute it to 100 mL. The valid period is 30 days.
5.3.6 Silver diethyldithiocarbamate-pyridine solution
Weigh 0.5 g of silver diethyldithiocarbamate. Dissolve it in 100 mL of pyridine. This
solution is stored in a brown bottle in a cool place. It is valid for one week.
Arabic. Add 250 mL of water. Warm to dissolve it. Add 87.0 g of ammonium acetate.
After dissolving, add 145 mL of 5% hydrochloric acid solution. Dilute it to 500 mL.
Filter if necessary. The valid period is one month.
5.3.15 Phenylanthranilic acid-ethanol solution (1 g/L)
Weigh 0.10 g of phenylanthranilic acid. Dissolve it in ethanol. Use ethanol, to dilute it
to 100 mL.
5.3.16 Benzoylphenylhydroxylamine solution (20 g/L)
Weigh 2.0 g of benzoylphenylhydroxylamine (tantalum reagent). Dissolve it in ethanol.
Use ethanol, to dilute it to 100 mL.
5.3.17 Phenylfluorenone solution (0.1 g/L)
Weigh 0.010 g of phenylfluorenone. Dissolve it in an appropriate amount of warm
ethanol. Add 1 mL of 20% hydrochloric acid solution Use ethanol, to dilute it to 100
mL.
5.3.18 Potassium hydroxide-ethanol solution
Weigh 30 g of potassium hydroxide. Dissolve it in 30 mL of water. Use aldehyde-free
ethanol, to dilute it to 1000 mL. Store it in polyethylene plastic bottles. Let it stand for
24 h. Take the supernatant for use.
5.3.19 Potassium hydroxide-methanol solution
Mix 15.0 mL of 330 g/L potassium hydroxide solution. Mix it with 50 mL of carbonyl-
free methanol solution. The valid period is two weeks.
5.3.20 Ammonia solution
2.5% ammonia solution (w = 2.5%): Measure 103 mL of ammonia water; mix with 898
mL of water.
10% ammonia solution (w= 10%): Measure 400 mL of ammonia water; mix with 601
mL of water.
5.3.21 Hydrochloric acid solution
5% hydrochloric acid solution (w = 5%): Measure 120 mL of hydrochloric acid; mix
with 895 mL of water.
10% hydrochloric acid solution (w = 10%): Measure 245 mL of hydrochloric acid; mix
it with 776 mL of water.
15% hydrochloric acid solution (w = 15%): Measure 375 mL of hydrochloric acid; mix
with 651 mL of water.
20% hydrochloric acid solution (w = 20%): Measure 510 mL of hydrochloric acid; mix
with 516 mL of water.
5.3.22 Phenylhydrazine hydrochloride solution (10 g/L)
Weigh 1 g of phenylhydrazine hydrochloride. Dissolve in water. Dilute it to 100 mL.
Prepare it before use.
5.3.23 Ferrous-ferrous mixed solution
Weigh 10.0 g of ferrous ammonium sulfate [(NH4)2Fe(SO4)2 • 6H2O] and 1.0 g of ferric
ammonium sulfate [NH4Fe(SO4)2 • 12H2O]. Dissolve it in water. Add 5 mL of 20%
sulfuric acid solution. Dilute it to 100 mL.
5.3.24 Starch-zinc iodide solution
Solution I: Weigh 2.0 g of soluble starch. Mix it with 20 mL of water. Pour it into 200
mL of boiling water. Add 10.0 g of zinc chloride. Dissolve it.
Solution II: Weigh 0.50 g of metal zinc powder and 1.0 g of iodine. Add 10 mL of water.
Stir it, until the yellow color disappears. Filter it. Boil the filtrate. Cool it down.
Pour the solution II into the cooled solution I. Mix well. Dilute it to 500 mL. Store it in
a brown bottle. The valid period is one week.
Measure 1 mL of starch-zinc iodide solution, which is prepared by the above method.
Add 50 mL of water and 3 mL of sulfuric acid solution (1 + 5). Mix well. The solution
shall not show blue. Add 1 drop of potassium iodate solution [c(1/6KIO3) = 0.01 mol/L]
to the solution. Mix well. It shall produce blue immediately.
5.3.25 Mixed alkalis
Mix 2 volumes of 100 g/L sodium hydroxide solution with 1 volume of 100 g/L
anhydrous sodium carbonate solution.
5.3.26 1,10-phenanthroline (o-phenanthroline) solution
1,10-phenanthroline solution (2 g/L): Weigh 0.20 g of 1,10-phenanthroline (C12H8N2 •
H2O) or 1,10-phenanthroline hydrochloride (C12H8N2 • HCl • H2O). Add a small
amount of water. Shake until it is dissolved (heat if necessary). Dilute it to 100 mL.
1,10-phenanthroline solution (5 g/L): Weigh 0.50 g of 1,10-phenanthroline (C12H8N2 •
H2O) or 1,10-phenanthroline hydrochloride (C12H8N2 • HCl • H2O). Dissolve it in acetic
acid-sodium acetate buffer solution, which has pH ≈ 3. Use acetic acid-sodium acetate
buffer solution, which has pH ≈ 3, to dilute it to 100 mL.
5.3.32 Nitric acid solution
13% nitric acid solution (w = 13%): Measure 150 mL of nitric acid; mix with 863 mL
of water.
20% nitric acid solution (w = 20%): Measure 240 mL of nitric acid; mix with 780 mL
of water.
25% nitric acid solution (w = 25%): Measure 308 mL of nitric acid; mix with 715 mL
of water.
5.3.33 Silver nitrate solution (17 g/L)
Weigh 1.70 g of silver nitrate. Dissolve it in water. Dilute it to 100 mL. Store it in a
brown reagent bottle. Store it in the dark.
5.3.34 Ammonium sulfide solution
Measure 100 mL of carbon dioxide-free ammonia water. Pass in hydrogen sulfide gas,
until the solution turns yellow.
5.3.35 Sulfuric acid solution
0.5% sulfuric acid solution (w = 0.5%): Measure 2.8 mL of sulfuric acid; slowly pour
it into 978 mL of water; cool and mix it.
5% sulfuric acid solution (w = 5%): Measure 29 mL of sulfuric acid; slowly pour it into
966 mL of water; cool and mix it.
20% sulfuric acid solution (w = 20%): Measure 128 mL of sulfuric acid; slowly pour it
into 889 mL of water; cool and mix it.
40% sulfuric acid solution (w = 40%): Measure 294 mL of sulfuric acid; slowly pour it
into 752 mL of water; cool and mix it.
5.3.36 Copper sulfate solution (20 g/L)
Weigh 2 g of copper sulfate (CuSO4 • 5H2O). Dissolve it in water. Add 2 drops of
sulfuric acid. Dilute it to 100 mL.
5.3.37 Ferrous sulfate solution (50 g/L)
Weigh 5.0 g of ferrous sulfide (FeSO4 • 7H2O). Dissolve it in an appropriate amount of
water. Add 10 mL of sulfuric acid. Dilute it to 100 mL.
5.3.38 Ammonium ferrous sulfate solution (100 g/L)
Weigh 10.0 g of ammonium ferrous sulfate [(NH4)2Fe(SO4)2 • 6H2O]. Dissolve it in an
appropriate amount of water. Add 10 mL of sulfuric acid. Dilute it to 100 mL.
5.3.39 Manganese sulfate mixture
Weigh 67.0 g of manganese sulfate (MnSO4 • H2O). Dissolve it in 500 mL of water.
Add 138 mL of phosphoric acid and 130 mL of sulfuric acid. Dilute it to 1000 mL.
5.3.40 Silver sulfate solution (10 g/L)
Weigh 1.0 g of silver sulfate. Dissolve it in 50 mL of 40% sulfuric acid solution. Dilute
it to 100 mL.
5.3.41 Potassium sulfate ethanol solution
Take 0.020 g potassium sulfate. Dissolve it in (3 + 7) ethanol solution. Use (3 + 7)
ethanol solution, to dilute it to 100 mL.
5.3.42 Ammonium purpurate solution (0.5 g/L)
Weigh 0.050 g of ammonium purpurate. Dissolve it in water. Dilute it to 100 mL.
Prepare this solution before use.
5.3.43 Bromine solution [c (1/2Br2) = 0.1 mol/L]
5.3.43.1 Preparation
Weigh 25.0 g of potassium bromide. Dissolve it in 150 mL of water. Add 1.2 mL ~ 1.3
mL (4 g) of bromine. Dilute it to 500 mL. Store it in a plastic bottle.
5.3.43.2 Calibration
Pipette 25.00 mL of the above solution. Pour it into a 250 mL iodine volumetric flask.
Add 2.0 g of potassium iodide and 30 mL of water. Seal with water. Shake gently until
the potassium iodide is dissolved. Place it in a dark place for 5 min. Use sodium
thiosulfate standard titration solution [c (Na2S2O3) = 0.1 mol/L] to titrate it. When
approaching the end point, add 3 mL of 10 g/L starch indicator solution. Continue to
titrate, until the blue color of the solution disappears.
The concentration of bromine solution c (l/2Br2), expressed in mol/L, it calculated
according to formula (1):
Where:
V1 - The value of the volume of the standard titration solution of sodium thiosulfate,
which is consumed when the titration reaches the end point, in milliliters (mL);
Solution 2: Weigh 60 g of citric acid; dissolve it in a mixed solution of 150 mL of water
and 85 mL of nitric acid.
Solution 3: Slowly add solution 1 to solution 2, while stirring.
Solution 4: Add 5 mL of quinoline, to a mixture of 35 mL of nitric acid and 100 mL of
water.
Solution 5: Add solution 4 to solution 3; stir evenly; let it stand for 24 hours; filter it;
add 280 mL of acetone to the filtrate; use water to dilute it to 1000 mL; mix well.
Warning: This solution shall be kept in polyethylene bottles. This solution contains
acetone AND shall not be used near flames. If heating or boiling is required during
operation, it must be operated in a fume hood.
5.3.51 Sodium tetraphenylboron solution
Sodium tetraphenylboron solution (15 g/L): Weigh 15 g of sodium tetraphenylboron
[NaB(C6H5)4]. Dissolve it in 960 mL of water. Add 4 mL of 400 g/L sodium hydroxide
solution and 20 mL of 100 g/L magnesium chloride (MgCl2 • 6H2O) solution. Stir it for
15 min. Let it stand for 24 h. Use filter paper to filter it. Store the solution in a brown
bottle or a polyethylene bottle. If turbidity is found within one month, it shall be filtered
before use.
Sodium tetraphenylboron solution (10 g/L): Weigh 10 g of sodium tetraphenylboron
[NaB(C6H5)4] in a 500 mL beaker. Add about 300 mL of water to dissolve it. Add 2 g
of aluminum hydroxide or aluminum trichloride (if the solution is colored, add 2 g of
activated carbon to decolorize). Stir for 10 min. Use slow filter paper to filter it. If the
filtrate is cloudy at first, it is filtered again, until it is clear. All the filtrate is collected
in a 1000 mL volumetric flask. Add 2 mL of 200 g/L sodium hydroxide solution. Dilute
it to the mark. Mix well. Let it stand for 48 h, for later use.
Sodium tetraphenylboron washing solution (1.5 g/L): Use 10 parts volume water, to
dilute 1 part volume 15 g/L sodium tetraphenylboron solution.
Sodium tetraphenylboron washing solution (1 g/L): Use 10 parts volume water, to dilute
1 part volume 10 g/L sodium tetraphenylboron solution.
5.3.52 Sodium tetraphenylboron ethanol solution (34 g/L)
Weigh 3.4 g of sodium tetraphenylboron. Dissolve it in 100 mL of absolute ethanol.
Filter it.
5.3.53 Potassium tetraphenylboron ethanol saturated solution
5.3.53.1 Preparation of potassium tetraphenylboron
Weigh 0.2 g of potassium carbonate, accurate to 0.001 g. Dissolve it in 300 mL of water.
Add 5 drops of methyl red indicator solution. Use (1 + 9) acetic acid solution, to adjust
to red. Heat to 40 °C, on a water bath. Add 45 mL of sodium tetraphenylboron ethanol
solution, under stirring. Let it stand for 10 min. Remove and cool to room temperature.
Use a glass sand crucible, which has a clean filter plate aperture of 5 μm ~ 15 μm, to
perform suction filtration. Use (1 + 19) ethanol solution, to wash it. Transfer the
precipitate. Drain it. Remove the glass sand crucible. Use 10 mL of anhydrous ethanol,
to wash along the glass sand crucible wall, for three times. Drain it.
5.3.53.2 Saturated solution of potassium tetraphenylboron ethanol
In the prepared potassium tetraphenylboron, add 50 mL of ethanol and 950 mL of water.
Fully shake to make it saturated. Dry filter it before use.
5.3.54 Sodium sulfide solution
Method 1: Weigh 5 g of sodium sulfide; dissolve it in a mixed solution of 10 mL of
water and 30 mL of glycerol.
Method 2: Weigh 5 g of sodium hydroxide; dissolve it in a mixed solution of 30 mL of
water and 90 mL of glycerol. Cool half the volume of the solution, whilst lead in
hydrogen sulfide gas, to make it saturated; then add the second half to mix it. This
solution shall be protected from light, sealed and stored in a brown bottle. It is valid for
three months, after preparation.
5.3.55 Strychnine solution (50 g/L)
Weigh 5.0 g of strychnine. Dissolve in glacial acetic acid. Use glacial acetic acid, to
dilute it to 100 mL.
WARNING: This material is highly toxic and shall be handled with care, to
prevent ingestion. If inhaled, seek medical attention immediately.
5.3.56 Sodium chloride saturated solution saturated with acetylene
In 200 mL of saturated sodium chloride solution (375 g/L), add 2 drops of methyl
orange indicator solution (1 g/L). Use hydrochloric acid solution (1 + 99), to acidify it,
until the solution turns red. Then lead in acetylene gas to saturate it.
5.3.57 Lead acetate saturated solution (200 g/L)
Dissolve 50 g of lead acetate [Pb(CH3COO)2 • 3H2O], in 250 mL of water.
5.3.58 Potassium and sodium tartrate alkaline solution (50 g/L)
Weigh 50 g of sodium potassium tartrate (NaKC4H4O6 • 4H2O). Dissolve it in water.
Add 40 g of sodium hydroxide. Dilute it to 1000 mL (it should not be stored in a glass
bottle with a ground stopper).
......
 
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