GB/T 37354-2019 PDF in English
GB/T 37354-2019 (GB/T37354-2019, GBT 37354-2019, GBT37354-2019)
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Analytical method of chemical composition for activated carbon mercury removal catalyst
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Standards related to (historical): GB/T 37354-2019
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GB/T 37354-2019: PDF in English (GBT 37354-2019) GB/T 37354-2019
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 71.100.99
G 74
Analytical method of chemical composition for
activated carbon mercury removal catalyst
ISSUED ON: MARCH 25, 2019
IMPLEMENTED ON: FEBRUARY 01, 2020
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 General provisions ... 4
4 Sampling ... 5
5 Determination of sulfur (S) mass fraction ... 5
6 Determination of calcium (Ca) mass fraction - Atomic absorption
spectrophotometry ... 7
7 Determination of magnesium (Mg) mass fraction - Atomic absorption
spectrophotometry ... 9
8 Determination of iron (Fe) mass fraction - Atomic absorption
spectrophotometry ... 10
9 Determinations of mass fractions of calcium (Ca), magnesium (Mg), iron (Fe),
aluminum (Al) - Inductively coupled plasma emission spectroscopy ... 12
Analytical method of chemical composition for
activated carbon mercury removal catalyst
WARNING - Some reagents used in this Standard are toxic or corrosive,
and some operations are dangerous. This Standard does not reveal all
possible safety issues. Users shall exercise caution and have the
responsibility to take appropriate safety and health measures when
operating.
1 Scope
This Standard specifies the analytical method of chemical composition for
activated carbon mercury removal catalyst.
This Standard is applicable to the determinations of mass fractions of sulfur (S),
calcium (Ca), magnesium (Mg), iron (Fe), aluminum (Al) in activated carbon
mercury removal catalyst.
2 Normative references
The following referenced documents are indispensable for the application of
this document. For dated references, only the edition cited applies. For undated
references, the latest edition of the referenced document (including any
amendments) applies.
GB/T 602, Chemical reagent - Preparations of stock standard solutions
GB/T 603, Chemical reagent - Preparations of reagent solutions for use in
test methods
GB/T 6003.1, Test sieves - Technical requirements and testing - Part 1: Test
sieves of metal wire cloth
GB/T 6679, General rules for sampling solid chemical products
GB/T 6682, Water for analytical laboratory use - Specification and test
methods
3 General provisions
All reagents and water used in this Standard, when no other requirements are
Mix the sample and the mixed flux well and burn, to make all sulfur into soluble
sulfate. Add barium chloride solution to make sulfate to generate barium sulfate
precipitation. According to the mass of barium sulfate, calculate the content of
sulfur in the sample.
5.2 Reagents
5.2.1 Mixed flux: Take 2-portion masses of light magnesium oxide and 1-portion
mass of anhydrous sodium carbonate. Mix well and grind well. Store in a sealed
container.
5.2.2 Hydrochloric acid solution: 1+1.
5.2.3 Barium chloride solution: 100g/L.
5.2.4 Silver nitrate solution: 10g/L. 1g of silver nitrate is dissolved in 100mL of
water. Add 2~3 drops of nitric acid. Store in a brown bottle.
5.2.5 Methyl orange indicator liquid: 2g/L.
5.3 Test steps
5.3.1 Weigh about 0.2g of specimen (see 4.2), to the nearest of 0.0001g. Place
in a 50mL porcelain crucible. Add 2g of mixed flux. Mix well. Add 1g of mixed
flux on top. Place the crucible in a muffle furnace. Within 1h~2h, gradually heat
it from room temperature to 800°C~850°C. And remain 1h at this temperature.
Take it out to cool to room temperature. Use a glass rod to carefully stir the
burning matter in the crucible to loosen. Then move the burning matter into a
400mL beaker. Use hot water to rinse the inner wall of the crucible. Combine
the washing liquid into the beaker. Then add 100mL~150mL of distilled water
that has just boiled. Stir completely.
5.3.2 Use medium-speed qualitative filter paper to filer by the pouring method.
Use hot water to rinse 3 times. Then move the residues into the filter paper. Use
hot water to carefully wash at least 10 times. The total volume of the washing
liquid is about 250mL~300mL. Add 2~3 drops of methyl orange indicator into
the filtrate. Add hydrochloric acid solution to make the filtrate turn from yellow
to red and exceed by 2mL. Heat the solution till it is boiling. Under continuous
stirring, slowly add 15mL of barium chloride solution. And keep it 2h under the
slight boiling condition. The final solution volume is about 200mL. After the
solution is cooled or left overnight, use a slow-speed quantitative filter paper to
filter. Then use hot water to wash till it is chloride-free (when silver nitrate
solution is tested without turbidity). Move the filter paper that has precipitation
into a porcelain crucible with a known mass. After ash the filter pater at a low
temperature, burn in an 850°C~900°C muffle furnace for 40min. Take out the
porcelain crucible. Put into a dryer to cool to room temperature then weigh.
Atomic absorption spectrophotometer: with hollow calcium cathode lamp.
6.4 Test steps
6.4.1 Drawing of working curve
6.4.1.1 Take 5 pieces of 100mL volumetric flasks. Respectively add 0mL,
1.00mL, 2.00mL, 3.00mL, 4.00mL of calcium standard solution. In each
volumetric flask, respectively add 2mL of strontium chloride solution and 2mL
of hydrochloric acid solution. Use water to dilute to the scale. Shake well.
6.4.1.2 According to the operating conditions of the instrument, use air-
acetylene flame, use the blank solution that does not have calcium standard
solution to perform zero adjustment. At a wavelength of 422.7nm, determine
the absorbance of solution.
6.4.1.3 Take the mass concentration of calcium in the above solution (in
micrograms per milliliter) as the abscissa and the corresponding absorbance
value as the ordinate, to draw the working curve or calculate the linear
regression equation.
6.4.2 Determination
Weigh 10.00mL of test material solution. Place in a 50mL volumetric flask. Add
1mL of strontium chloride solution. Use water to dilute to the scale. Shake well.
According to the provisions of 6.4.1.2, determine the absorbance of the solution.
Find the mass concentration of calcium in the test solution from the working
curve or calculate it by the linear regression equation.
6.5 Test data processing
Calcium (Ca) mass fraction w2 is calculated according to formula (2):
Where,
ρ1 - Numerical value of the mass concentration of calcium in the test solution
that is found from the working curve or calculated by the linear regression
equation, in micrograms per milliliter (µg/mL);
V1 - Numerical volume value of test material solution, in milliliters (mL);
m4 - Numerical value of distributed test material’s mass, in grams (g).
Take the arithmetic mean of two parallel determination results as the
micrograms per milliliter) as the abscissa and the corresponding absorbance
value as the ordinate, to draw the working curve or calculate the linear
regression equation.
7.4.2 Determination
Weigh 10.00mL of test material solution in a 100mL volumetric flask. Add 2mL
of strontium chloride solution. Use water to dilute to the scale. Shake well.
According to the provisions of 7.4.1.2, determine the absorbance of solution.
Find the mass concentration of magnesium in the test solution from the working
curve or calculate it from the linear regression equation.
7.5 Test data processing
Calculate magnesium (Mg) mass fraction w3 according to formula (3):
Where,
ρ2 - Numerical value of the mass concentration of magnesium in the test
solution that is found from the working curve or calculated by the linear
regression equation, in micrograms per milliliter (µg/mL);
V2 - Numerical volume value of test material solution, in milliliters (mL);
m5 - Numerical value of distributed test material’s mass, in grams (g).
Take the arithmetic mean of two parallel determination results as the
measurement result. The relative deviation of the parallel determination results
is not more than 5%.
8 Determination of iron (Fe) mass fraction - Atomic
absorption spectrophotometry
8.1 Principle
Under acidic conditions, use atomic absorption spectrophotometer, use air-
acetylene flame, at a wavelength of 248.3nm, to determine the absorbance of
iron in the test material solution. Use the working curve method or the linear
regression equation to quantify.
8.2 Reagents
m6 - Numerical value of test material’s mass, in grams (g).
Take the arithmetic mean of two parallel determination results as the
measurement result. The relative deviation of the parallel determination results
is not more than 5%.
9 Determinations of mass fractions of calcium (Ca),
magnesium (Mg), iron (Fe), aluminum (Al) - Inductively
coupled plasma emission spectroscopy
9.1 Principle
Under acidic conditions, use high purity argon flame to introduce the solution
atomization into inductively coupled plasma. Determine the signal intensity of
the analytical lines of calcium, magnesium, iron, and aluminum in the test
material solution. Use the working curve method to quantify.
9.2 Reagents
9.2.1 Hydrochloric acid solution: 1+1.
9.2.2 Calcium standard solution: 0.1mg/mL.
9.2.3 Magnesium standard solution: 0.1mg/mL.
9.2.4 Iron standard solution: 0.1mg/mL.
9.2.5 Aluminum standard solution: 0.1mg/mL.
9.3 Instruments
Inductively coupled plasma emission spectrometer.
9.4 Test steps
9.4.1 Drawing of working curve
9.4.1.1 Take 5 pieces of 100mL volumetric flasks. Respectively pipette
corresponding standard solution. Prepare standard solution series according to
Table 1. In each volumetric flask, respectively add 2mL of hydrochloric acid
solution. Use water to dilute to the scale. Shake well.
......
Source: Above contents are excerpted from the PDF -- translated/reviewed by: www.chinesestandard.net / Wayne Zheng et al.
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