GB/T 603-2023 English PDF (GB/T603-2023)

GB/T 603-2023: Chemical reagent - Preparations of reagent solutions for use in test methods
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GB/T 603-2023
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 71.040.40; 71.040.30
CCS G 60
Replacing GB/T 603-2002
Chemical Reagent - Preparations of Reagent Solutions for
Use in Test Methods
(ISO 6353-1:1982, Reagents for Chemical Analysis - Part 1: General Test Methods,
NEQ)
ISSUED ON: AUGUST 6, 2023
IMPLEMENTED ON: MARCH 1, 2024
Issued by: State Administration for Market Regulation;
Standardization Administration of the People’s Republic of China.
Table of Contents
Foreword ... 3
1 Scope ... 6
2 Normative References ... 6
3 Terms and Definitions ... 6
4 General Provisions ... 6
5 Preparation Methods ... 7
Index ... 34
Chemical Reagent - Preparations of Reagent Solutions for
Use in Test Methods
1 Scope
This document specifies the preparation methods for reagent solutions for use in test methods
of chemical reagent.
This document is applicable to the preparation of preparations and products required for
chemical reagent analysis. It can also be used in other fields.
2 Normative References
The contents of the following documents constitute indispensable clauses of this document
through the normative references in the text. In terms of references with a specified date, only
versions with a specified date are applicable to this document. In terms of references without a
specified date, the latest version (including all the modifications) is applicable to this document.
GB/T 601 Chemical Reagent - Preparations of Standard Volumetric Solutions
GB/T 602 Chemical Reagent - Preparations of Standard Solutions for Impurity
GB/T 6682 Water for Analytical Laboratory Use - Specification and Test Methods
GB/T 9733 Chemical Reagent - General Method for the Determination of Carbonyl Compounds
3 Terms and Definitions
This document does not have terms or definitions that need to be defined.
4 General Provisions
4.1 Unless otherwise specified in this document, the reagents used shall be of analytically pure
(including analytically pure) or above. The standard titration solutions and standard solutions
used shall be prepared in accordance with the stipulations of GB/T 601 and GB/T 602. The test
water shall comply with the specifications of Grade-3 water in GB/T 6682, and the reagents
shall be weighed accurately to 0.01 g or measured accurately to 0.1 mL.
4.2 Unless otherwise specified in this document, all solvents not specified are water.
4.3 The test solution (A + B) involved in this document refers to solute A and solvent B that are
1---acid solution;
2---reaction reagent;
3---water;
4---sodium hydroxide solution (100 g/L);
A---dropping funnel;
B---reaction bottle;
C---washing bottle;
D---absorption bottle;
E---safety bottle;
F---exhaust gas absorption bottle.
Figure 1 -- Preparation Device for Saturated Sulfur Dioxide Solution and Saturated
Hydrogen Sulfide Water
5.1.1.2 Saturated hydrogen sulfide water
In the fume hood, as shown in Figure 1, connect the device. Add hydrochloric acid solution
(20%) to A, and add ferrous sulfide to B. The hydrochloric acid solution (20%) is dripped from
A into B, and the generated hydrogen sulfide gas is passed into carbon dioxide-free water, until
the D solution is saturated (the mass no longer increases).
Hydrogen sulfide gas can be prepared with a commercially available hydrogen sulfide gas
generator, or hydrogen sulfide cylinder gas can be used and directly introduced into C.
5.1.1.3 Saturated bromine water
In the fume hood, measure-take 10 mL of bromine, add it to a brown bottle filled with 75 mL
of water, shake it well, and place it for stratification. The supernatant liquid is saturated bromine
water.
5.1.1.4 Aqua regia
Slowly pour 1 volume of nitric acid into 3 volumes of hydrochloric acid and mix it well. Prepare
it just before use.
5.1.1.5 Ammonia-free sodium hydroxide solution
Pour the sodium hydroxide solution of the required concentration into the flask and boil it for
30 minutes. Tighten the rubber stopper of a double-ball safety funnel containing sulfuric acid
solution (20%) and cool (as shown in Figure 2) and use ammonia-free water to dilute it to the
original volume.
5.1.1.12 Oxygen-free water
Pour water into a flask, boil for 1 h and immediately use a rubber stopper equipped with a glass
delivery tube to tightly plug it. The tube is connected to a washing bottle containing pyrogallic
acid alkaline solution (100 g/L) and cooled. The usage period is 2 days.
5.1.2 Test solution
5.1.2.1 Ammonia solution
5.1.2.1.1 Ammonia solution (2.5%)
Measure-take 103 mL of ammonia water and dilute to 1,000 mL.
5.1.2.1.2 Ammonia solution (10%)
Measure-take 400 mL of ammonia water and dilute to 1,000 mL.
5.1.2.2 Phenyl anthranilic acid-ethanol solution (1 g/L)
Weigh-take 0.1 g of phenyl anthranilic acid, dissolve it in ethanol (95%), and use ethanol (95%)
to dilute to 100 mL.
5.1.2.3 Phenylfluorone solution (0.1 g/L)
Weigh-take 0.01 g (accurate to 0.0001 g) of phenylfluorone (benzofluorenone), add an
appropriate amount of ethanol (95%), warm to dissolve it; add 1 mL of hydrochloric acid
solution (20%), and use ethanol (95%) to dilute to 100 mL.
5.1.2.4 Benzoylphenylhydroxylamine solution (20 g/L)
Weigh-take 2 g of benzoyl phenyl hydroxylamine (tantalum reagent), dissolve it in ethanol
(95%), and use ethanol (95%) to dilute to 100 mL. The usage period is 6 months.
5.1.2.5 Benzopenttrione color developer
5.1.2.5.1 Benzopenttrione-acetone color developer
Weigh-take 2 g of benzopenttrione (ninhydrin), dissolve it in acetone, and use acetone to dilute
to 100 mL. Place it in a brown bottle. The usage period is 14 days.
5.1.2.5.2 Benzopenttrione-ethanol color developer
Weigh-take 4 g of benzopenttrione (ninhydrin), dissolve it in ethanol (absolute ethanol), and
use ethanol (anhydrous ethanol) to dilute to 1,000 mL. Place it in a brown bottle. The usage
period is 2 months.
5.1.2.6 Ammonium pyrrolidine dithiocarbamate (APDC) solution (10 g/L)
Weigh-take 1 g of ammonium pyrrolidine dithiocarbamate (APDC), dissolve it in water, dilute
to 100 mL, if necessary, filter it.
5.1.2.7 Chromotropic acid solution (5 g/L)
Weigh-take 0.5 g of chromotropic acid, dissolve it in an appropriate amount of water, dilute to
100 mL and shake it well; use a slow filter paper to filter it. Prepare it just before use.
5.1.2.8 Oxalic acid solution (50 g/L)
Weigh-take 5 g of oxalic acid dihydrate (oxalic acid), dissolve it in water, and dilute to 100 mL.
5.1.2.9 Titan yellow solution (0.5 g/L)
Weigh-take 0.05 g (accurate to 0.0001 g) of titan yellow, dissolve it in water, and dilute to 100
mL. The usage period is 3 months.
5.1.2.10 Starch-potassium iodide solution
In 100 mL of newly prepared starch indicator solution (10 g/L), add 0.2 g of potassium iodide
and dissolve it. Prepare it just before use.
5.1.2.11 Starch-zinc iodide solution
Solution I: weigh-take 2 g of soluble starch and mix it with 20 mL of water, pour it into 200 mL
of boiling water, add 10 g of zinc chloride, and dissolve it.
Solution II: weigh-take 0.5 g of metal zinc powder and 1 g of iodine, add 10 mL of water, stir
it, until the yellow color disappears, and filter it. Boil the filtrate and cool it.
Pour Solution II into the cooled Solution I, mix it well, and dilute to 500 mL. Place it in a brown
bottle. The usage period is 7 days.
The starch-zinc iodide solution prepared in accordance with the above-mentioned method shall
satisfy the following requirements: measure-take 1 mL of starch-zinc iodide solution, add 50
mL of water and 3 mL of sulfuric acid solution (1 + 5), and mix it well; the solution shall not
appear blue. Add 1 drop of potassium iodate standard titration solution [c(ଵ଺KIO3) = 0.01 mol/L]
into the solution, mix it well, and blue color shall immediately appear.
5.1.2.12 Sodium indigo disulfonate solution [c(C16H8N2Na2O8S2) = 0.001 mol/L]
5.1.2.12.1 Preparation
Weigh-take sodium indigo disulfonate (indigo carmine), add 2 mL of sulfuric acid solution (1
+ 5) to dissolve it, and dilute to 1,000 mL. The usage period is 10 days.
The mass m of sodium indigo disulfonate required to prepare sodium indigo disulfonate solution
[c(C16H8N2Na2O8S2) = 0.001 mol/L], expressed in (g), is calculated in accordance with Formula
Weigh-take 0.3324 g of 4,7-diphenyl-1,10-phenanthroline, dissolve it in ethanol (95%), and use
ethanol (95%) to dilute to 1,000 mL.
5.1.2.15 2,4-dinitrophenylhydrazine solution (1 g/L)
Weigh-take 0.1 g of 2,4-dinitrophenylhydrazine, dissolve it in 50 mL of carbonyl-free methanol
and 4 mL of hydrochloric acid, and dilute to 100 mL. The usage period is 14 days.
5.1.2.16 Sodium diethyldithiocarbamate solution (1 g/L)
Weigh-take 0.1 g of sodium diethyldithiocarbamate (copper reagent), dissolve it in water, and
dilute to 100 mL. The usage period is 1 month.
5.1.2.17 Silver diethyldithiocarbamate-pyridine solution (5 g/L)
Weigh-take 0.5 g of silver diethyldithiocarbamate and use pyridine to dilute it to 100 mL. Place
it in a brown bottle and store in a cool place. The usage period is 7 days.
5.1.2.18 Silver diethyldithiocarbamate-triethylamine chloroform solution
Weigh-take 0.25 g of silver diethyldithiocarbamate, use a small amount of chloroform to
dissolve it, add 1.8 g of triethylamine, and use chloroform to dilute to 100 mL. Let it stand
overnight, then filter it. Place it in a brown bottle and store it away from light. The usage period
is 7 days.
5.1.2.19 1,10-phenanthroline solution
5.1.2.19.1 1,10-phenanthroline solution (2 g/L)
Weigh-take 0.20 g of 1,10-phenanthroline (C12H8N2  H2O) [or 0.24 g of 1,10-phenanthroline
hydrochloride (C12H8N2  HCl  H2O)], add a small amount of water and shake it, until it is
dissolved (if necessary, heat it), then, dilute to 100 mL.
5.1.2.19.2 1,10-phenanthroline solution (5 g/L)
Weigh-take 0.5 g of 1,10-phenanthroline (C12H8N2  H2O) [or 0.6 g of 1,10-phenanthroline
hydrochloride (C12H8N2  HCl  H2O)], dissolve it in acetic acid-sodium acetate buffer solution
(pH  3), and use acetic acid-sodium acetate buffer solution (pH  3) to dilute to 100 mL.
5.1.2.20 Fehling’s solution
Solution I: weigh-take 34.7 g of copper (II) sulfate pentahydrate (copper sulfate), dissolve it in
water, and dilute to 500 mL.
Solution II: weigh-take 173 g of sodium potassium tartrate tetrahydrate (potassium sodium
tartrate) and 50 g of sodium hydroxide, dissolve it in water, and dilute to 500 mL.
During use, mix Solution I and Solution II in the same volume.
5.1.2.21 Potassium fluoride solution (58 g/L)
Weigh-take 94 g of potassium fluoride dihydrate (potassium fluoride), dissolve it in water, and
dilute to 1,000 mL. Place it in a polyethylene bottle.
5.1.2.22 Griess reagent
Solution I: weigh-take 0.1 g of methyl naphthylamine, add 100 mL of water, boil to dissolve
and cool it. Add 3 mL of acetic acid (glacial acetic acid) and shake it well. Place it in a brown
bottle. The usage period is 3 months.
Solution II: weigh-take 1 g of anhydrous p-aminobenzene sulfonic acid, dissolve in water and
dilute to 100 mL. The usage period is 3 months.
During use, mix Solution I and Solution II in the same volume.
5.1.2.23 Chromic acid solution (100 g/L)
Weigh-take 100 g of chromium trioxide, dissolve it in sulfuric acid solution (35%), and use
sulfuric acid solution (35%) to dilute it to 1,000 mL.
5.1.2.24 Chrome azurol S mixture
Solution I: weigh-take 0.5 g of cetyltrimethylammonium bromide, dissolve it in water and dilute
to 100 mL.
Solution II: weigh-take 0.04 g (accurate to 0.0001 g) of chrome azurol S, add 5 mL of ethanol
(95%) to dissolve it and dilute to 100 mL.
Take 10 mL of Solution I and 50 mL of Solution II, and dilute to 100 mL.
5.1.2.25 5-sulfosalicylic acid solution (100 g/L)
Weigh-take 10 g of 5-sulfosalicylic acid dihydrate (5-sulfosalicyclic acid), dissolve it in water
and dilute to 100 mL.
5.1.2.26 Mixed base
Take 200 mL of sodium hydroxide solution (100 g/L), add 100 mL of anhydrous sodium
carbonate solution (100 g/L) and mix it well.
5.1.2.27 Alkaline fuchsin-sulphurous acid solution
Sodium sulfite solution (100 g/L): weigh-take 2 g of sodium sulfite heptahydrate and dissolve
it in 20 mL of water.
Weigh-take 0.2 g of basic fuchsin, dissolve it in 120 mL of hot water, cool it, then, add 20 mL
of sodium sulfite solution (100 g/L), add 2 mL of hydrochloric acid and dilute to 200 mL, let it
stand for 1 hour.
5.1.2.32 Quin molybdenum ketone solution
Solution I: weigh-take 70 g of sodium molybdate dihydrate and dissolve it in 150 mL of water.
Solution II: weigh-take 60 g of citric acid monohydrate (citric acid) and dissolve it in a mixture
of 150 mL of water and 85 mL of nitric acid.
Solution III: while stirring, slowly add Solution I to Solution II.
Solution IV: add 5 mL of quinoline to a mixture of 35 mL of nitric acid and 100 mL of water.
Solution V: add Solution IV to Solution III, evenly stir it, and let it stand for 24 hours. Use a
glass filter crucible or filter paper to filter it. Add 280 mL of acetone to the filtrate, dilute to
1,000 mL, and mix it well. Place it in a polyethylene bottle and store it in a dark place away
from light and heat. The usage period is 6 months. During use, operate in a fume hood and keep
it away from fire sources.
5.1.2.33 Phosphorus reagent A
Weigh-take 5 g of ammonium molybdate tetrahydrate (ammonium molybdate), dissolve it in
water and dilute to 100 mL. Place it in a polyethylene bottle. If precipitation is found, it shall
be prepared again.
5.1.2.34 Phosphorus reagent B
Weigh-take 0.2 g of paramethylaminophenol sulfate (metol), dissolve it in 100 mL of water,
add 20 g of sodium metabisulfite (sodium metabisulfite), and dissolve it. Place it in a
polyethylene bottle and store it away from light. The usage period is 14 days.
5.1.2.35 Sodium dihydrogen phosphate solution (200 g/L)
Weigh-take 20 g of sodium dihydrogen phosphate dihydrate (sodium dihydrogen phosphate),
dissolve it in water, add 1 mL of sulfuric acid solution (20%) and dilute to 100 mL.
5.1.2.36 Thioacetamide mixture