Some standard content:
ICS 71. 060. 30
Record number: 7509-2000
HG/T3687—2000
This standard is formulated based on the requirements of domestic and foreign users and the actual level of industrial sodium hydrosulfide production in my country. This standard combines the characteristics of domestic industrial sodium hydrosulfide enterprise standards to divide products into two categories: solid and liquid. Liquid products are divided into two specifications of 36% and 28%. The indicators of solid superior products are better than the actual measured data of foreign products. The test methods for sodium hydrosulfide content and sodium sulfide content basically adopt HG/T29644—1984 "Sodium Hydrosulfide Test Method", and supplement the arbitration method of the end point of the acidometer indication to solve the problem that the first end point of some products is not obvious enough. The test method for iron content is added. Since the requirements for iron content cannot be unified for the time being, it is stipulated that the iron content index shall be implemented by agreement. This standard is proposed by the Policy and Regulations Department of the State Administration of Petroleum and Chemical Industry. This standard is under the jurisdiction of the Inorganic Chemical Branch of the National Chemical Standardization Technical Committee. This standard was drafted by: Tianjin Chemical Research and Design Institute, Henan Shanxian Huayuan Barium Salt Factory, Tianjin Organic Chemical Plant No. 1. The main drafters of this standard are: Fan Guoqiang, Fan Zhanyin, Gao Xizhi, Wang Chuntiao. This standard is entrusted to the Inorganic Chemical Branch of the National Technical Committee for Chemical Standardization for interpretation. This standard is published for the first time.
Chemical Industry Standard of the People's Republic of China
Industrial Sodium Hydrosulfide
Sodium hydrosulfide for industrial useHG/T3687—2000
This standard specifies the requirements, test methods, inspection rules, marking, labeling, packaging, transportation and storage of industrial sodium hydrosulfide. This standard is applicable to block, flake, granular and liquid industrial sodium hydrosulfide, which is mainly used in mineral processing, pesticides, leather making, dye production and organic synthesis industries.
Molecular formula NaHS·H,O
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 are subject to revision. Parties using this standard should explore the possibility of using the latest versions of the following standards. GB190—1990 Dangerous Goods Packaging Marking
GB/T601--1988 Preparation of Standard Solutions for Titration Analysis (Volume Analysis) of Chemical Reagents Preparation of Standard Solutions for Determination of Impurities of Chemical Reagents GB/T 602—1988
GB/T 603—1988
GB/T 1250—1989
GB/T 3049--1986
GB/T6682--1992
3 Classification
Preparation of preparations and products used in chemical reagent test methods Methods for expressing and determining limit values General method for determining iron content in chemical products O-phenanthroline spectrophotometry (negISO6685:1982)
Specifications and test methods for water used in analytical laboratories (neqISO3696:1987) This standard divides industrial sodium hydrosulfide products into two categories: liquid and solid: liquid products are divided into two specifications of 36% and 28%. Requirements
Appearance: solid is yellow, orange-yellow, brown, gray-brown block, granular, or flake; liquid is light yellow, green-yellow or orange-red tortoise. 4.1
Industrial sodium hydrosulfide should meet the requirements of Table 1.
Table 1 Requirements
Sodium hydrosulfide (NaHS) content ≥
Sodium sulfide (NazS) content
Iron content
Superior quality
Approved by the State Administration of Petroleum and Chemical Industry on 2000-08-21
First-class quality
Qualified quality
Implemented on 2001-05-01
5 Test methods
HG/T 3687—2000
The reagents and water used in this standard, unless otherwise specified, refer to analytical reagents and grade 3 water specified in GB/T6682. The standard titration solutions, impurity standard solutions, preparations and products used in the test, unless otherwise specified, are prepared in accordance with the provisions of GB/T601, GB/T602 and GB/T603.
Safety Tips: The strong acids and alkalis used in this standard are corrosive. Be careful when operating to avoid splashing. The hydrogen sulfide released during the test is harmful to human health and flammable. Be careful to operate in a fume hood. 5.1 Determination of sodium hydrosulfide content and sodium sulfide content 5.1.1 Method Summary
After the sample is dissolved, add barium chloride to remove carbonate, fix the volume, and dry filter. Remove the filtrate and titrate with hydrochloric acid standard titration solution. Use an indicator or acidometer to indicate the end point and calculate the sodium sulfide content; add formaldehyde to react with sodium hydrosulfide to release sodium hydroxide. Use phenolic acid as an indicator to continue titrating with hydrochloric acid to the end point and calculate the sodium hydrosulfide content. 5.1.2 Reagents and Materials
5.1.2.1 Formaldehyde: 36% 38%. Filter with medium-speed filter paper before use. Use phenolic acid indicator solution and drop sodium hydroxide standard titration solution [c(HCI) about 0.1 mol/L] until the solution turns slightly red. 5.1.2.2 Barium chloride solution: 100 g/L.
5.1.2.3 Hydrochloric acid standard titration solution: c(HCI) about 0.1 mol/L. 5.1.2.4 Phenolic acid indicator solution: 1% ethanol solution. 5.1.2.5 Alizarin yellow GG-thymol blue mixed indicator solution: a) 0.1 g Alizarin yellow GG is dissolved in 100 mL 50% ethanol solution. b) 0.1 g thymol blue is dissolved in 100 mL 50% ethanol solution. c) Take 30 ml a) and 20 mL b) and mix. 5.1.3 Instruments and equipment
Acidity meter: accuracy is 0.02 pH unit, equipped with calomel electrode and glass electrode. 5.1.4 Analysis steps
5.1.4.1 Preparation of test solution
Use a weighing bottle with known mass to weigh about 12g of liquid sample or 6g of solid sample (accurate to 0.001g). Transfer all to a 500mL volumetric flask with 15ml of barium chloride solution. Add a small amount of water to dissolve, shake the hook, and let it stand for 10min. Dilute with water to the scale and mix well. Use medium-speed filter paper for dry filtration, discard 20mL of the initial filtrate, and collect the filtrate in a dry 500mL conical flask. The amount of filtrate is enough for the test, and the rubber stopper is covered. This solution is solution A. The mass (m) of the sodium hydrosulfide solid sample sampled from the barrel is calculated according to formula (1): m=m2×ms
Wherein: mi—
-mass of the prepared total solution, kg;
-net mass of the barrel of sodium hydrosulfide, kg;
-mass of the total solution sample weighed with a weighing bottle, kg. mg
-5.1.4.2 Determination
Pipette 25mL of solution A and place it in a 250mL conical flask, add 20mL of water, and add 10 drops of alizarin yellow GG-thymol blue mixed indicator solution. Titrate with hydrochloric acid standard titration solution. The end point is when the solution changes from green to blue (if the end point is not obvious, it can be indicated by an acidometer, and pH=9.8 is the end point. This method is used for arbitration). Then add 5mL of formaldehyde and 3 drops of phenolic acid indicator solution, and continue to titrate with hydrochloric acid standard titration solution. The end point is when the red color of the solution disappears completely. 5.1.5 Expression of analysis results
5.1.5.1 The sodium hydrosulfide (NaHS) content (X) expressed as mass fraction shall be calculated according to formula (2): 1136
Wherein: V.
HG/T 3687--2000
(V - 2V,)sX 0. 056 06 ×100
m×500
The volume of the standard hydrochloric acid titration solution consumed when titrating to the first endpoint, mL; V,—the total volume of the standard hydrochloric acid titration solution consumed when titrating to the second endpoint, mL; The actual concentration of the standard hydrochloric acid titration solution, mol/L; 0. 056 06
The mass of sodium hydrosulfide equivalent to 1.00mL of standard hydrochloric acid titration solution [Ec(HClI)-1.000mol/L], expressed in grams;
The mass of the sample, g.
5.1.5.2 The sodium sulfide (NaaS) content (X2) expressed as mass fraction is calculated according to formula (3): X = Yic×0.978 04 ×100
m×500
Wherein: V, the volume of the hydrochloric acid standard titration solution consumed when titrating to the first endpoint, mL; the actual concentration of the hydrochloric acid standard titration solution, mol/L; (3)
0.078 04 ---
mass of sodium sulfide in grams equivalent to 1.00mL of the hydrochloric acid standard titration solution [c(HC1)=1.000mol/L];
m-mass of the sample, g.
5.1.6 Allowable difference
The arithmetic mean of the parallel determination results is taken as the determination result. The absolute difference of the parallel determination results: sodium hydrosulfide is not more than 0.3%, and sodium sulfide is not more than 0.1%.
5.2 Determination of iron content
5.2.1 Summary of method
After the sample is dissolved in water, sulfuric acid is added and heated in an electric furnace to decompose sodium hydrosulfide. It is burned at 600℃ in a high-temperature furnace to completely decompose polysulfide and sulfur. The iron in the residue is dissolved with hydrochloric acid, and the trivalent iron is reduced to divalent iron with ascorbic acid. In the pH range of 2 to 9, divalent iron and o-phenanthroline form a red complex, and the absorbance is measured by a spectrophotometer at the maximum absorption wavelength (510nm). 5.2.2 Reagents and materials
Same as Chapter 3 of GB/T3049-1986 and
Sulfuric acid solution: 1+5.
5.2.3 Instruments and equipment
Same as Chapter 4 of GB/T3049-1986 and
Ceramic crucible: 50mL.
5.2.4 Analysis steps
5.2.4.1 Drawing of working curve
Draw the working curve according to the provisions of 5.3 of GB/T3049-1986. 5.2.4.2 Determination
Weigh about 10g of sample (accurate to 0.01g). Add appropriate amount of water to dissolve and transfer to a 100mL volumetric flask, dilute with water to the scale, and shake well. Immediately transfer 10ml, weigh about 2g of liquid sample directly, and place it in a 50mL porcelain crucible. Add 4mL of sulfuric acid solution in a fume hood. Place the crucible on an electric furnace and heat until the sulfuric acid is driven out. Place the crucible in a high-temperature furnace and burn at 600℃ for 10min. Cool, add 1mL of 1+1 hydrochloric acid solution and appropriate amount of water, and heat to dissolve the residue. After cooling, transfer the solution to a 100mL volumetric flask and operate the test solution according to the provisions of 5.4 of GB/T3049-1986, starting from "add water to about 60mL when necessary". The blank solution is without adding sample, and the amount of other reagents added is the same as when treating the sample. 5.2.5 Expression of analysis results
The iron (Fe) content (X.) expressed as mass fraction is calculated according to formula (4): 1137
HG/T 3687-2000
(ml-mo)X 10-
× 100 bZxz.net
mi-mo
Where: m.---the mass of iron found from the working curve according to the measured absorbance of the test solution, mg; mo-the mass of iron found from the working curve according to the measured absorbance of the air start solution, mg; m-the mass of the sample. . .
5.2.6 Allowable difference
The arithmetic mean of the parallel determination results is taken as the determination result. The relative deviation of the two parallel determination results shall not exceed 20%. 6 Inspection rules
6.1 All items specified in this standard are factory inspection items and must be inspected batch by batch. 6.2 Each batch of products shall not exceed 60t.
6.3 See Table 2 for sampling methods.
Total number of product packages (barrels or bags)
1~100
101~200
Number of sampling packages (barrels or bags)
6.3.1 Sampling of solid products for complete dissolution: Select packaging units according to Table 2 for complete dissolution sampling, cut open the selected packages, crush the samples, quickly pour them into a dissolution tank of known weight, weigh the mass of sodium hydrosulfide, and then add water to dissolve. Steam heating can be used to accelerate dissolution. After complete dissolution, continue to add water to make a solution with a mass fraction of about 30% and weigh its mass. The following operation is also applicable to liquid products. Under continuous stirring, use a glass tube with an inner diameter of 10mm~15mm and a tip, insert it to 2/3 at a speed at which the liquid levels inside and outside the tube are level, and take out a total of not less than 300g of liquid sample. Immediately pack into clean, dry wide-mouth bottles or plastic bottles and seal them. Stick a label on the bottle, indicating: manufacturer name, product name, batch number, sampling date and name of the sampler, for inspection on the same day. 6.3.2 The manufacturer can take representative liquid samples during the packaging of solid products and make solid samples after cooling. Conduct the test directly. When there is a quality dispute between the supply and demand parties, the results of the full dissolution sampling test shall prevail. 6.4 Industrial sodium hydrosulfide shall be inspected by the quality supervision and inspection department of the manufacturer in accordance with the provisions of this standard. The manufacturer shall ensure that each batch of products leaving the factory meets the requirements of this standard.
6.5 The user has the right to inspect and accept the industrial sodium hydrosulfide received in accordance with the provisions of this standard. The inspection and acceptance shall be carried out within one month from the date of arrival of the goods.
6.6 If one of the indicators in the inspection results does not meet the requirements of this standard, re-sampling from twice the amount of packaging shall be conducted for re-inspection. Even if only one indicator in the re-inspection results does not meet the requirements of this standard, the entire batch of products shall be unqualified. 6.7 The rounded value comparison method specified in GB/T1250 shall be used to determine whether the test results meet the standard. 7 Marking and labeling
7.1 The packaging of industrial sodium hydrosulfide shall be firmly and clearly marked, including: manufacturer name, factory address, product name, trademark, net content, grade, this standard number and the "corrosive product" mark specified in GB190. 7.2 Each batch of products leaving the factory shall be accompanied by a quality certificate. The contents include: manufacturer name, factory address, product name, trademark, net content, grade, batch number or production date, proof that the product quality meets this standard and this standard number. 8 Packaging, transportation, storage
8.1 Solid industrial sodium hydrosulfide is packaged in iron drums or other packaging forms required by users and in accordance with storage and transportation safety regulations. The net contents are 25kg, 50kg or 150kg respectively; liquid products are shipped in iron drums or tank trucks, with a net content of 200kg per barrel. 1138
HG/T3687---2000
8.2 Industrial sodium hydrosulfide products should be stored in a cool, dry, ventilated warehouse, protected from rain, moisture, heat, and should not come into contact with acids and corrosive substances.
8.3 During transportation, industrial sodium hydrosulfide products should be protected from sunlight, rain, and heat, and the packaging should be kept intact. 8.4 The shelf life of industrial sodium hydrosulfide is 1 year at room temperature of 20°C, relative humidity not exceeding 60%, and the packaging kept intact. 11393 Sampling method See Table 2.
Total number of product packages (barrels or bags)
1~100
101~200
Number of sampling packages (barrels or bags)
6.3.1 Sampling of full dissolution of solid products: Select the packaging unit according to Table 2 for full dissolution sampling, cut open the selected package, crush the sample, quickly pour it into a dissolution tank of known weight, weigh the mass of sodium hydrosulfide and then add water to dissolve. Steam heating can be used to accelerate the dissolution. After the dissolution is complete, continue to add water to make a solution with a mass fraction of about 30% and weigh its mass. The following operation is also applicable to liquid products. Under continuous stirring, use a glass tube with an inner diameter of 10mm~15mm and a tip, insert it to 2/3 at a speed at which the liquid levels inside and outside the tube are level, and take out a total of not less than 300g of liquid sample. Immediately pack into clean, dry wide-mouth bottles or plastic bottles and seal them. Stick a label on the bottle, indicating: manufacturer name, product name, batch number, sampling date and name of the sampler, for inspection on the same day. 6.3.2 The manufacturer can take representative liquid samples during the packaging of solid products and make solid samples after cooling. Conduct the test directly. When there is a quality dispute between the supply and demand parties, the results of the full dissolution sampling test shall prevail. 6.4 Industrial sodium hydrosulfide shall be inspected by the quality supervision and inspection department of the manufacturer in accordance with the provisions of this standard. The manufacturer shall ensure that each batch of products leaving the factory meets the requirements of this standard.
6.5 The user has the right to inspect and accept the industrial sodium hydrosulfide received in accordance with the provisions of this standard. The inspection and acceptance shall be carried out within one month from the date of arrival of the goods.
6.6 If one of the indicators in the inspection results does not meet the requirements of this standard, re-sampling from twice the amount of packaging shall be conducted for re-inspection. Even if only one indicator in the re-inspection results does not meet the requirements of this standard, the entire batch of products shall be unqualified. 6.7 The rounded value comparison method specified in GB/T1250 shall be used to determine whether the test results meet the standard. 7 Marking and labeling
7.1 The packaging of industrial sodium hydrosulfide shall be firmly and clearly marked, including: manufacturer name, factory address, product name, trademark, net content, grade, this standard number and the "corrosive product" mark specified in GB190. 7.2 Each batch of products leaving the factory shall be accompanied by a quality certificate. The contents include: manufacturer name, factory address, product name, trademark, net content, grade, batch number or production date, proof that the product quality meets this standard and this standard number. 8 Packaging, transportation, storage
8.1 Solid industrial sodium hydrosulfide is packaged in iron drums or other packaging forms required by users and in accordance with storage and transportation safety regulations. The net contents are 25kg, 50kg or 150kg respectively; liquid products are shipped in iron drums or tank trucks, with a net content of 200kg per barrel. 1138
HG/T3687---2000
8.2 Industrial sodium hydrosulfide products should be stored in a cool, dry, ventilated warehouse, protected from rain, moisture, heat, and should not come into contact with acids and corrosive substances.
8.3 During transportation, industrial sodium hydrosulfide products should be protected from sunlight, rain, and heat, and the packaging should be kept intact. 8.4 The shelf life of industrial sodium hydrosulfide is 1 year at room temperature of 20°C, relative humidity not exceeding 60%, and the packaging kept intact. 11393 Sampling method See Table 2.
Total number of product packages (barrels or bags)
1~100
101~200
Number of sampling packages (barrels or bags)
6.3.1 Sampling of full dissolution of solid products: Select the packaging unit according to Table 2 for full dissolution sampling, cut open the selected package, crush the sample, quickly pour it into a dissolution tank of known weight, weigh the mass of sodium hydrosulfide and then add water to dissolve. Steam heating can be used to accelerate the dissolution. After the dissolution is complete, continue to add water to make a solution with a mass fraction of about 30% and weigh its mass. The following operation is also applicable to liquid products. Under continuous stirring, use a glass tube with an inner diameter of 10mm~15mm and a tip, insert it to 2/3 at a speed at which the liquid levels inside and outside the tube are level, and take out a total of not less than 300g of liquid sample. Immediately pack into clean, dry wide-mouth bottles or plastic bottles and seal them. Stick a label on the bottle, indicating: manufacturer name, product name, batch number, sampling date and name of the sampler, for inspection on the same day. 6.3.2 The manufacturer can take representative liquid samples during the packaging of solid products and make solid samples after cooling. Conduct the test directly. When there is a quality dispute between the supply and demand parties, the results of the full dissolution sampling test shall prevail. 6.4 Industrial sodium hydrosulfide shall be inspected by the quality supervision and inspection department of the manufacturer in accordance with the provisions of this standard. The manufacturer shall ensure that each batch of products leaving the factory meets the requirements of this standard.
6.5 The user has the right to inspect and accept the industrial sodium hydrosulfide received in accordance with the provisions of this standard. The inspection and acceptance shall be carried out within one month from the date of arrival of the goods.
6.6 If one of the indicators in the inspection results does not meet the requirements of this standard, re-sampling from twice the amount of packaging shall be conducted for re-inspection. Even if only one indicator in the re-inspection results does not meet the requirements of this standard, the entire batch of products shall be unqualified. 6.7 The rounded value comparison method specified in GB/T1250 shall be used to determine whether the test results meet the standard. 7 Marking and labeling
7.1 The packaging of industrial sodium hydrosulfide shall be firmly and clearly marked, including: manufacturer name, factory address, product name, trademark, net content, grade, this standard number and the "corrosive product" mark specified in GB190. 7.2 Each batch of products leaving the factory shall be accompanied by a quality certificate. The contents include: manufacturer name, factory address, product name, trademark, net content, grade, batch number or production date, proof that the product quality meets this standard and this standard number. 8 Packaging, transportation, storage
8.1 Solid industrial sodium hydrosulfide is packaged in iron drums or other packaging forms required by users and in accordance with storage and transportation safety regulations. The net contents are 25kg, 50kg or 150kg respectively; liquid products are shipped in iron drums or tank trucks, with a net content of 200kg per barrel. 1138
HG/T3687---2000
8.2 Industrial sodium hydrosulfide products should be stored in a cool, dry, ventilated warehouse, protected from rain, moisture, heat, and should not come into contact with acids and corrosive substances.
8.3 During transportation, industrial sodium hydrosulfide products should be protected from sunlight, rain, and heat, and the packaging should be kept intact. 8.4 The shelf life of industrial sodium hydrosulfide is 1 year at room temperature of 20°C, relative humidity not exceeding 60%, and the packaging kept intact. 1139
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