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GB/T 23978-2020 English PDF (GBT23978-2020)

GB/T 23978-2020 English PDF (GBT23978-2020)

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GB/T 23978-2020: Determination of chloride in water-soluble dyes
GB/T 23978-2020
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 71.100.01; 87.060.10
G 55
Replacing GB/T 23978-2009
Determination of chloride in water-soluble dyes
ISSUED ON: NOVEMBER 19, 2020
IMPLEMENTED ON: OCTOBER 01, 2021
Issued by: State Administration for Market Regulation;
Standardization Administration of the People’s Republic of
China.
Table of Contents
Foreword ... 3 
1 Scope ... 4 
2 Normative references ... 4 
3 Determination methods ... 4 
4 Test report ... 9 
Appendix A (Informative) Ion chromatogram for the determination of chloride in
water-soluble dyes ... 10 
Determination of chloride in water-soluble dyes
1 Scope
This Standard specifies the determination method of chloride in water-soluble
dyes.
This Standard applies to various water-soluble dyes.
2 Normative references
The following documents are indispensable for the application of this document.
For dated references, only the dated version applies to this document. For
undated references, the latest edition (including all amendments) applies to this
document.
GB/T 601, Chemical reagent - Preparations of reference titration solutions
GB/T 603, Chemical reagent - Preparations of reagent solutions for use in
test methods
GB/T 6682-2008, Water for analytical laboratory use - Specification and test
methods (ISO 3696:1987, MOD)
GB/T 8170-2008, Rules of rounding off for numerical values and expression
and judgement of limiting values
3 Determination methods
3.1 Ion chromatography
3.1.1 Determination principle
For the pre-treated water-soluble dye sample solution, use the ion
chromatography, with retention time for qualitative determination and peak area
external standard method for quantitative determination, to determine its
chloride content (as NaCl).
3.1.2 General provisions
Unless otherwise specified, use only reagents that are identified as analytical
reagents, and grade-3 water that is specified in GB/T 6682-2008. The
Burn the sodium chloride at 500 °C to a constant amount; then, weigh about
1.000 g (accurate to 0.000 1 g) in a 1 000 mL volumetric flask; add water to
dissolve and dilute to a constant volume; prepare a sodium chloride solution
whose concentration is 1 000 μg/mL. Then, prepare linear standard solutions
of seven concentrations of 0.01 μg/mL, 0.05 μg/mL, 0.1 μg/mL, 0.5 μg/mL, 1.0
μg/mL, 5.0 μg/mL, and 10.0 μg/mL for use.
3.1.8 Determination
After the instrument is running stably, use a syringe to respectively draw the
standard solution and sample solution to fill the quantitative loop for injection.
After the chloride ion peak has flowed out (see Figure A.1 in Appendix A), use
the chromatographic workstation to process the results. Determine the peak
area of sodium chloride in the standard solution; draw a standard curve; then,
calculate the chloride content in the sample according to the standard curve.
3.1.9 Result calculation
The standard curve equation of sodium chloride is calculated according to
Formula (1):
The content of chloride (calculated as NaCl) in the sample is calculated, as
mass fraction w1 (%), according to Formula (2):
Where:
A -- peak area value of sodium chloride;
k -- constant of the sodium chloride standard curve equation, which is given by
the chromatographic workstation;
ρ -- concentration of sodium chloride in the solution, in micrograms per milliliter
(μg/mL);
b -- constant of the sodium chloride standard curve equation, which is given by
the chromatographic workstation;
V1 -- value of the final constant volume of the sample solution, in milliliters (mL);
n -- value of the dilution ratio of the sample;
m1 -- value of the mass of the sample, in grams (g);
3.2.3.2 Nitric acid.
3.2.3.3 Nitric acid solution: the volume ratio of nitric acid to water = 1:1.
3.2.3.4 Nitrobenzene.
3.2.3.5 Silver nitrate standard titration solution: c(AgNO3) = 0.1 mol/L.
3.2.3.6 Ferric ammonium sulfate test solution: Weigh 14 g of ferric ammonium
sulfate; dissolve it in 100 mL of water; filter; add 10 mL of nitric acid; store in a
brown bottle; place it in a refrigerator. The validity period is 6 months.
3.2.3.7 Ammonium thiocyanate standard titration solution: c(NH4SCN) = 0.1
mol/L.
3.2.4 Preparation of sample solution
Weigh about 2 g (accurate to 0.000 1 g) of the sample; dissolve it in 150 mL of
water; add 15 g of activated carbon; gently boil for 2 min ~ 3 min. Cool to room
temperature; add 1 mL of nitric acid solution; place for 30 min (shake it
occasionally). Use a Buchner funnel for suction filtration. If the filtrate is colored,
add another 5 g of activated carbon; place for 1 h while shaking it from time to
time; then, use a Buchner funnel for suction filtration (if there is still color,
replace the activated carbon and repeat the operation until the filtrate is
colorless). Use 10 mL of water to wash the activated carbon 3 times; combine
and transfer the filtrate to a 250 mL volumetric flask; use water to fix volume;
shake well; set aside.
3.2.5 Determination steps
Pipette 50.00 mL of the sample solution (3.2.4); place it in a 250 mL conical
flask; add 2 mL of nitric acid solution (3.2.3.3), 10.00 mL of silver nitrate
standard titration solution (3.2.3.5) and 5 mL of nitrobenzene; vigorously shake
until the silver chloride precipitates and coagulates; add 1 mL of ferric
ammonium sulfate test solution; use the ammonium thiocyanate standard
titration solution to titrate the excess silver nitrate; the solution changes from
light yellow to light red as the end point; keep it for 1 min. Do a blank test at the
same time.
Note: If the chloride content is high, and the chloride ion in the sample cannot
be completely precipitated with 10.00 mL of silver nitrate standard
titration solution, dilute the sample solution.
3.2.6 Result calculation
The content of chloride (calculated as NaCl) in the sample is calculated, as
mass fraction w2 (%), according to Formula (3):

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