Some standard content:
HG/T 2778—1996
This standard is formulated based on relevant foreign data and combined with my country's actual situation, thus providing a unified technical basis for pure hydrochloric acid in my country's chemical industry.
The technical requirements of this standard are divided into first-class products and qualified products. This standard sets requirements for six items: total acidity, iron, calcium, magnesium, free fluorine, and evaporation residue. The test methods are all general methods. This standard is proposed by the Technical Supervision Department of the Ministry of Chemical Industry of the People's Republic of China. This standard is technically managed by the Jinxi Chemical Research Institute of the Ministry of Chemical Industry. The responsible drafting units of this standard: Jinxi Chemical Research Institute of the Ministry of Chemical Industry, Tangshan Jidong Chemical Plant. The main drafters of this standard; Wang Lanfang, Guan Liping, Zheng Zhiguo, Hu Liming, Wang Zhifang, Zhang Fengqin, Miao Aijun. This standard was first issued in 1996.
1 Scope
Chemical Industry Standard of the People's Republic of China
High Purity Hydrochloric Acid
HG/T 2778—1996
This standard specifies the requirements, sampling, test methods, and marking, labeling, packaging, and safety requirements for high-purity hydrochloric acid. This product is used for the adjustment of the pH value of the anode liquid of ion membrane caustic soda electrolysis, the regeneration of resin towers, and the production and application of high-purity products such as medicines. Molecular formula: HCI
Relative molecular mass: 36.45 (according to the 1991 international relative atomic mass) 2 Referenced standards
The provisions contained in the following standards constitute the provisions of this standard through reference in this standard. When this standard is published, the versions shown are valid. All standards will be screened and revised, and parties using this standard should explore the possibility of using the latest versions of the following standards. GB190—1990 Dangerous Goods Packaging Marking
GB320-1993 Synthetic Hydrochloric Acid for Industrial Use
3 Preparation of Standard Solutions for Chemical Reagents for Full Quantity Analysis (Volumetric Analysis)GB/T 601--1988
GB/T 602—1988
GB/T 603--1988
GB/T 1250—1989
GB/T 6678—1986
GR/T 6680—1986
GB/T 6682-1992
3 Requirements
Preparation of standard solutions for determination of impurities in chemical reagents (neqISO6353-1:1982) Preparation of preparations and products used in test methods for chemical reagents (neqIS06353-1:1982) Expression and determination methods of limit values General rules for sampling of chemical products
General procurement for sampling of liquid chemical products
Specifications and test methods for water in analytical laboratories (e9vIS03696:1987) Appearance: colorless or slightly yellowish transparent liquid. 3.1
High purity hydrochloric acid shall meet the requirements of Table 1:
Table 1 Requirements for high purity hydrochloric acid
Total acidity (in HCI), %
Calcium (in Ca), mg/L
Iron (in Fe), mg/L
Evaporation residue, mg/L
Free oxygen, m/L
Approved by the Ministry of Chemical Industry of the People's Republic of China on January 24, 1996 520
Qualified products
Implemented on January 1, 1997
4 Sampling
HG/T 2778-1996
4. 1 The product is batched into each storage tank (tank) or tank truck. When the product is stored and transported in plastic barrels, it shall be in accordance with GB/T 6678 6.6 The number of sampling units shall be determined according to the provisions of the standard. When sampling, take equal amounts of samples from the top, middle and bottom of different depths, mix and pack them into two clean, dry glass bottles with ground stoppers. Each bottle shall not be less than 500 mL. One bottle is for inspection and one bottle is for retention sample. The retention period is one month. The bottle is labeled with the manufacturer's name, product name, batch number, sampling date and name of the sampler. 4.2 If one of the indicators does not meet the requirements of this standard, the sample should be re-taken from two packages for verification. If even one of the indicators does not meet the requirements of this standard, the whole batch of products cannot be accepted. 5 Test method
All items specified in this standard are type inspection items, among which total acidity, calcium, iron, magnesium and free fluoride are output inspection items. Type inspection is carried out once a week.
This standard adopts the correction value comparison method specified in GB/T1250 to determine whether the inspection results meet the standard. Unless otherwise specified, the reagents used in this standard are analytically pure reagents, and the water used should comply with the third-grade water specified in GB/T6682. The standard titration solutions, impurity standard solutions, preparations and products used shall be prepared in accordance with the provisions of GB/T601, GB/T602 and GB/T603 unless otherwise specified.
5.1 Determination of total acidity
Determine in accordance with 4.1 of GB 320.
5.2 Determination of calcium, magnesium and iron content - flame atomic absorption spectrophotometry (extension method) 5.2.1 Summary of the method
Determine the absorbance of the treated test solution by flame atomic absorption spectrometry, and quantify by the standard curve method. 5.2.2 Reagents or materials
When determining, use high-purity reagents and double distilled water or water of corresponding purity made from quartz glass containers. 5.2.2.1 Hydrochloric acid solution; 1+1;
5.2.2.2 Strontium fluoride solution: 45 g/L
Weigh 76.1 g SrCl, -6H,0 and dissolve in water, dilute to 1 000 mL. 5.2.2.3 Calcium standard solution: 10 μg/mL
Dilute the solution prepared according to GB/T602 10 times. 5.2.2.4 Magnesium standard solution, 5 μg/ml.1Dilute the solution prepared according to GB/T602 20 times. 5.2.2.5 Iron standard solution: 10 μg/mL; Dilute the solution prepared according to GB/T602 10 times. 5.2.3 Instruments and equipment
5.2.3.1 Flame-melting atomic absorption spectrophotometer; 5.2.3.2 Acetylene-air flame;
5.2.3.3 Instrument working conditions:
Wavelength, calcium (Ca) 422.7 nm
Magnesium (Mg) 285.2 nm;
Iron (Fe) 248.3 nm.
5.2.4 Analysis steps
5.2.4.1 Preparation of test solution
Usage: Measure 100 mL of hydrochloric acid sample into a 500 mL high-profile quartz beaker, heat on an electric furnace and concentrate to 1 mL~2 mL. Cool slightly, add 5 mL of hydrochloric acid solution and heat slowly to dissolve all residues. Cool to room temperature, add 5 mL of the healing solution, transfer the sample to a 25 mL volumetric flask, dilute to the mark with water, and perform a blank test at the same time. 5.2.4.2 Preparation of standard solutions
Add calcium, magnesium, and iron standard solutions to 7 25 mL volumetric flasks according to the amounts specified in Table 2, then add 5 mL of strontium chloride solution and 5 mL of hydrochloric acid solution, dilute to the mark with water, mix, and wait for measurement. Table 2 Amount of standard solution added
Amount of calcium standard solution added, mL
5.2.4.3 Preparation of standard curve
Amount of standard solution added, mL
Amount of standard solution added, mL
Absorb calcium, magnesium, and iron standard solutions into the flame in turn, and use calcium, magnesium, and iron hollow cathode lamps to measure their absorbances, respectively. With the measured absorbance as the ordinate and the concentration of calcium, magnesium and iron as the abscissa, draw the standard curves of calcium, magnesium and iron respectively (use double distilled water or water of corresponding purity to adjust to zero).
5.2.5 Sample determination
Absorb the sample solution into the flame, use the calcium, magnesium and iron hollow cathode lamps to measure their absorbance respectively, and find out the concentration of calcium, magnesium and iron on the standard curve prepared in advance according to the absorbance. 5.2.6 Expression of analysis results
5.2.6.1 Calcium (X) expressed in milligrams per liter (mg/L) is calculated according to formula (1): XI
Where a
(a-ar) × 25
The corresponding calcium concentration found on the standard curve, μg/mL; The calcium concentration in the blank found on the standard curve, μg/mL; The volume of the sample after treatment, mL;
100---The sample volume, mL.
5.2.6.2 Magnesium (X,) expressed in milligrams per liter (mg/L) is calculated according to formula (2): X
Where: 5
5.2. 6. 3
(b --br ) × 25
From the standard curve.t corresponding magnesium concentration, ug/mL; magnesium concentration in blank obtained from standard curve, μg/mL: volume of sample after treatment, mL;
sample crystal volume, mL.
Iron (X,) expressed in milligrams/liter (mg/L) is calculated according to formula (3): X,
(c ci) × 25
Where: - — corresponding iron concentration obtained from standard curve g/mL G1 - — iron concentration in blank obtained from standard curve, μg/mL; 25
- volume of sample after treatment, mL;
100 sample volume, mL.
（1）
（2）
5.2.7 Allowable difference
HG/T 2778—1996
Take the arithmetic mean of the results of two parallel determinations as the reported result. The absolute value of the difference between the two parallel determinations shall not exceed 0.01 mg/L (Ca); 0.004 mg/L (Mg); 0,008 mg/L (Fe). 5.3 Determination of calcium, magnesium and iron content
5.3.1 Summary of method
Inductively coupled plasma emission spectrometry
The spectral line intensity of each element in the treated test solution is determined by inductively coupled plasma emission spectrometry, and the standard addition method is used for quantification. 5.3.2 Reagents or materials
Sub-boiling water made of high-purity reagents and quartz glass is used for determination. 5.3.2.1 Calcium standard solution: 10 μg/mL; dilute 10 times the solution prepared according to GB/T 602. 5.3.2.2 Magnesium standard solution; 10 μg/mL; dilute 10 times the solution prepared according to GB/T 602. 5.3.2.3 Iron standard solution: 10 μg/mL; dilute 10 times the solution prepared according to GB/T 602. 5.3.3 Instruments and equipment
5.3.3.1 Inductively coupled plasma emission spectrometer (ICP instrument); 5.3.3.2 Volumetric flask: 100mL (made of polyethylene); 5.3.3.3 Pipette: 10mL (made of polyethylene). 5.3.3.4 Instrument working conditions
Test according to the optimal working conditions specified by different types of instruments in each unit. 5.3.4 Analysis steps
Use a pipette to transfer 10 mL of hydrochloric acid sample into a 100 mL volumetric flask and dilute to the mark with water. At the same time, transfer 10 mL of high-grade pure hydrochloric acid as a blank. 5.3.5 Determination of samples
Put the sample drop into the plasma and determine the concentrations of calcium, magnesium and iron respectively. 5.3.6 Expression of analysis results
5.3.6.1 Magnesium (X,) expressed in grams per liter (mg/L) is calculated according to formula (4): X -(a-ai) x10
Where: α-
Measured calcium concentration in the test sample: Hg/mL;
a: m Blank measured calcium concentration, μg/mL. 5.3. 6.2 Magnesium (X,) expressed in milligrams per liter (mg/L) is calculated according to formula (5): X = (b-b) × 10
Where: 6
- magnesium concentration in the sample, μg/mL; - magnesium concentration measured in the blank, μg/mL. br
5.3. 6.3 Iron (Xs) expressed in milligrams per liter (mg/L) is calculated according to formula (6): X = (c-) × 10
Where: c-
iron concentration in the sample, μg/mL;
cl- iron concentration measured in the blank, μg/mL. 5. 4 Determination of evaporation residue
5.4.1 Summary of the method
Evaporate a certain volume of sample to dryness, keep constant weight, and then weigh. 5.4.2 Instruments and equipment General laboratory instruments. - (4) \ (5) 5.4.3 Analytical procedures Pipette 100 mL of sample and place it in a weighed (accurate to 0.000 1 g) evaporating liquid which has been dried at 105°C to 110°C and weighed to a constant weight. Evaporate to dryness in a water bath, cool to room temperature in a desiccator, weigh to a constant weight at 105°C to 110°C, and weigh (accurate to 0.000 1 g). 5.4.4 Expression of analysis results
The evaporation residue (X,) expressed in milligrams per liter (mg/L) is calculated according to formula (7): 7)
Where: m
Mass of evaporation residue, mg!
V— -sample volume, L.
5.4.5 Allowable difference
The arithmetic mean of the two reverse determination results is taken as the reported result. The absolute value of the difference between the two parallel determination results shall not exceed 6 mg/1-. 5.5 Determination of free chlorine content
According to 4.6 of GB320
6 Marking, labeling, packaging
6.1 Marking
The packaging container of high-purity hydrochloric acid shall be firmly labeled with the following contents: the manufacturer’s name, address, product name, trademark, net weight, batch number or production date, the number of this standard and the “corrosive product mark” specified in GB190. 6.2 Labeling
Each batch of products leaving the factory shall be accompanied by a label, including: product name, quality grade, manufacturer’s name, address, trademark, production date Period, implementation standard number, storage and transportation precautions, safety matters, etc. 6.3 Packaging
When high-purity hydrochloric acid is packaged in polyvinyl chloride barrels or ceramic jars, the filling port should be covered with a screw cap, and the surrounding of the cap should be sealed with acid-resistant materials. It is then packed in wooden boxes or crates, and the box opening should be at least 20mm away from the filling port. When it is packaged in tank trucks and storage tanks, it should be lined with rubber and sealed with a cover. It must not be mixed with toxic or harmful items during transportation or storage. 7 Safety requirements
High-purity hydrochloric acid is a highly corrosive product. People who come into contact with it must wear protective equipment such as glasses and acid-resistant gloves. 524) is calculated according to formula (5): X = (b-b) × 10
where: 6
-the magnesium concentration in the sample, μg/mL; -the magnesium concentration in the blank, μg/mL. br
5.3. 6.3 Iron (Xs) expressed in milligrams/liter (mg/L) is calculated according to formula (6): X = (c-) × 10
where: c-
the iron concentration in the sample, μg/mL;
cl-the iron concentration in the blank, μg/mL. 5. 4 Determination of evaporation residue
5.4.1 Summary of the method
Evaporate a certain volume of sample to dryness, keep constant weight, and then weigh it. 5.4.2 Instruments and equipment
General laboratory instruments.
-（4）)
\（5)
5.4.3 Analysis steps
HG/T 2778--1996
Use a pipette to transfer 100 mL of sample, place it in a weighed (accurate to 0.000 1 g) evaporation liquid dried at 105℃～110℃ and constant weight, evaporate to dryness on a water bath, cool to room temperature in a desiccator, constant weight at 105℃～110℃, and weigh (accurate to 0.000 1 g). 5.4.4 Expression of analysis results
The evaporation residue (X,) expressed in milligrams/liter (mg/L) is calculated according to formula (7): 7)
Where: m
Mass of evaporation residue, mg!
V— -sample volume, L.
5.4.5 Allowable difference
Take the arithmetic mean of the two reverse determination results as the reported result. The absolute value of the difference between the two parallel determination results shall not exceed 6 mg/1-. 5.5 Determination of free chlorine content
According to 4.6 of GB320
6 Marking, labeling, packaging
6.1 Marking
A firm mark shall be affixed to the packaging container of high-purity hydrochloric acid, which shall include the manufacturer's name, address, product name, trademark, net weight, batch number or production date, number of this standard and the "corrosive product mark" specified in GB190. 6.2 Label
Each batch of products leaving the factory shall be accompanied by a label, which shall include: product name, quality grade, manufacturer's name, address, trademark, production date Period, implementation standard number, storage and transportation precautions, safety matters, etc. 6.3 Packaging
When high-purity hydrochloric acid is packaged in polyvinyl chloride barrels or ceramic jars, the filling port should be covered with a screw cap, and the surrounding of the cap should be sealed with acid-resistant materials. It is then packed in wooden boxes or crates, and the box opening should be at least 20mm away from the filling port. When it is packaged in tank trucks and storage tanks, it should be lined with rubber and sealed with a cover. It must not be mixed with toxic or harmful items during transportation or storage. 7 Safety requirements
High-purity hydrochloric acid is a highly corrosive product. People who come into contact with it must wear protective equipment such as glasses and acid-resistant gloves. 524) is calculated according to formula (5): X = (b-b) × 10
where: 6
-the magnesium concentration in the sample, μg/mL; -the magnesium concentration in the blank, μg/mL. br
5.3. 6.3 Iron (Xs) expressed in milligrams/liter (mg/L) is calculated according to formula (6): X = (c-) × 10
where: c-
the iron concentration in the sample, μg/mL;
cl-the iron concentration in the blank, μg/mL. 5. 4 Determination of evaporation residuebzxz.net
5.4.1 Summary of the method
Evaporate a certain volume of sample to dryness, keep constant weight, and then weigh it. 5.4.2 Instruments and equipment
General laboratory instruments.
-（4）)
\（5)
5.4.3 Analysis steps
HG/T 2778--1996
Use a pipette to transfer 100 mL of sample, place it in a weighed (accurate to 0.000 1 g) evaporation liquid dried at 105℃～110℃ and constant weight, evaporate to dryness on a water bath, cool to room temperature in a desiccator, constant weight at 105℃～110℃, and weigh (accurate to 0.000 1 g). 5.4.4 Expression of analysis results
The evaporation residue (X,) expressed in milligrams/liter (mg/L) is calculated according to formula (7): 7)
Where: m
Mass of evaporation residue, mg!
V— -volume of sample, L.
5.4.5 Allowable difference
Take the arithmetic mean of the two reverse determination results as the reported result. The absolute value of the difference between the two parallel determination results shall not exceed 6 mg/1-. 5.5 Determination of free chlorine content
According to 4.6 of GB320
6 Marking, labeling, packaging
6.1 Marking
A firm mark shall be affixed to the packaging container of high-purity hydrochloric acid, which shall include the manufacturer's name, address, product name, trademark, net weight, batch number or production date, number of this standard and the "corrosive product mark" specified in GB190. 6.2 Label
Each batch of products leaving the factory shall be accompanied by a label, which shall include: product name, quality grade, manufacturer's name, address, trademark, production date Period, implementation standard number, storage and transportation precautions, safety matters, etc. 6.3 Packaging
When high-purity hydrochloric acid is packaged in polyvinyl chloride barrels or ceramic jars, the filling port should be covered with a screw cap, and the surrounding of the cap should be sealed with acid-resistant materials. It is then packed in wooden boxes or crates, and the box opening should be at least 20mm away from the filling port. When it is packaged in tank trucks and storage tanks, it should be lined with rubber and sealed with a cover. It must not be mixed with toxic or harmful items during transportation or storage. 7 Safety requirements
High-purity hydrochloric acid is a highly corrosive product. People who come into contact with it must wear protective equipment such as glasses and acid-resistant gloves. 524
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