Some standard content:
HG/T 2827—1997
This standard is equivalent to the US military standard MIL-C-51264A:1983 (confirmed in 1989). Compared with MIL-C-51264A:1983 (confirmed in 1989), this standard has the following differences: 1 This standard divides industrial cuprous cyanide into two grades: superior and first-class. Superior is equivalent to MIL-C-51264A:1983 (confirmed in 1989).
2 This standard adds the main content index expressed by cuprous cyanide (CuCN) because of the usage habits and needs of most users. 3 This standard adds the iron content index, the purpose of which is to further ensure the intrinsic quality of the product in combination with domestic production conditions. 4 Except for the test method corresponding to the added iron content index, which adopts GB/T3049-1986, other test methods are equivalent to the corresponding methods of MIL-C-51264A:1983.
Appendix A of this standard is the appendix of the standard.
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 under the jurisdiction of Tianjin Chemical Research Institute of the Ministry of Chemical Industry. The drafting units of this standard are Tianjin Chemical Research Institute of the Ministry of Chemical Industry, Shanghai Dunhuang Chemical Plant, Shandong Zichuan Shuangfeng Chemical Plant, Zhejiang Xiaoshan Chemical Reagent Factory, and Tianjin Ruicheng Chemical Co., Ltd. The main drafters of this standard are Fan Guoqiang, Shen Jinxi, Shi Zuyu, Kong Qingwu, Xu Shuiming, and Yang Zhanzhou. This standard is entrusted to the technical unit responsible for the standardization of inorganic salt products of the Ministry of Chemical Industry for interpretation. 699
1 Scope
Chemical Industry Standard of the People's Republic of China
Cuprous cyanide
Cuprous cyanide for industrial useHG/T 2827--1997
This standard specifies the requirements, sampling, test methods, marking, packaging, transportation, storage and safety requirements for industrial cuprous cyanide. This standard is applicable to industrial cuprous cyanide, which is mainly used for cyanide electroplating. Molecular formula: CuCN
Relative molecular mass: 89.56 (according to the 1993 international relative atomic mass) 2 Reference 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 revised, and the parties using this standard should explore the possibility of using the latest versions of the following standards. GB190--1990 Dangerous Goods Packaging Marking
GB/T 601--1988
GB/T 602--1988
GB/T 603-1988
GB/T 1250-1989
Preparation of standard solutions for titration analysis (volume analysis) of chemical reagentsPreparation of standard solutions for determination of impurities of chemical reagents (neqISO6353-1:1982)Preparation of preparations and products used in test methods for chemical reagents (neqISO6353-1:1982)Expression and determination methods of limit valuesGB/T 3049--1986
GB/T 6678-1986
GB/T 6682—1992
3 Requirements
General method for determination of iron content in chemical products (1982)
General rules for sampling of chemical products
O-Phenylene spectrophotometric method (neqISO6685: Specifications and test methods for water used in analytical laboratories (eqyISO3696:1987) 3.1 Appearance: white, grayish yellow or sky blue powder or loose block. 3.2 Industrial cuprous cyanide shall meet the requirements of Table 1. Table
Copper (Cu) content
Content of cuprous cyanide (CuCN) (converted to Cu content) Content of cyanide (calculated as CN)
Insoluble matter in sodium cyanide
Content of iron (Fe)
Approved by the Ministry of Chemical Industry of the People's Republic of China on February 4, 1997 700
Superior product
First-class product
Implemented on October 1, 1997
4 Sampling
4.1 No more than 21 per batch of products.
HG/T 2827--1997
4.2 Determine the number of sampling units in accordance with the provisions of 6.6 in GB/T66781986. When sampling, use a sampler to obliquely insert from the top of the packaging barrel to 3/4 of the material layer to collect samples, mix the samples evenly, and use the quartering method to reduce them to about 250g. Immediately put them into two clean, dry large bottles and seal them. Attach labels to the bottles, indicating: manufacturer name, product name, grade, batch number, sampling date and name of the sampler. One bottle is used as a laboratory sample, and the other is kept for one month for future reference. 4.3 If one indicator of the test results does not meet the requirements of this standard, re-sample from twice the amount of packaging for verification. , even if only one indicator does not meet the requirements of this standard, the entire batch of products shall be deemed unqualified. 5 Test method
5.1 The rounded value comparison method specified in 5.2 of GB/T1250--1989 shall be used to determine whether the test results meet the standard. 5.2 The reagents and water used in this standard, unless otherwise specified, refer to analytical pure reagents and grade 3 water specified in GB/T6682-1992.
The standard titration solution, impurity standard solution, preparation and products used in the test, unless otherwise specified, shall be prepared in accordance with the provisions of GB/T601, GB/T602 and GB/T603.
5.3 Determination of copper (Cu) content
5.3.1 Summary of method
After the sample is decomposed by adding nitric acid and bromine water, it is adjusted to weak acidity with ammonia water and acetic acid. Add the masking agent potassium fluoride, add excess potassium iodide, titrate the released iodine with sodium thiosulfate standard titration solution, and use starch indicator to indicate the end point. 5.3.2 Reagents and Materials
5.3.2.1 Ammonia water;
5.3.2.2 Glacial acetic acid;
5.3.2.3 Potassium fluoride;
5.3.2.4 Potassium iodide;
5.3.2.5 Nitric acid solution: 1+3;
5.3.2.6 Saturated bromine aqueous solution;
5.3.2.7 Sodium thiosulfate standard titration solution: c(NazS,O.) is about 0.1mol/L; 5.3.2.8 Starch indicator solution: 10g/1.
5.3.3 Analysis steps
Weigh about 0.3g of sample (accurate to 0.0001g). Place in a 250mL conical flask and operate in a fume hood. Add 10ml nitric acid solution and heat until hydrogen cyanide and nitrogen oxides are completely removed; add 5mL saturated bromine water and continue heating for 5min until the bromine gas is completely driven out. Dilute to 25ml with cold water, add ammonia water dropwise to neutralize until blue appears, add 5ml glacial acetic acid, cool to 10℃±2℃, add 0.5g potassium fluoride and 20g potassium iodide, and shake well. Titrate the solution with sodium thiosulfate standard titration solution until light brown or yellow color almost disappears, add 5ml starch indicator solution, and continue titrating the solution until the blue color disappears as the end point. Perform a blank test at the same time. 5.3.4 Expression of analysis results
The copper content X expressed as mass percentage is calculated according to the formula (1): X = 0.0636×(V/-Ve)c×100m
Wherein: V,—
the volume of sodium thiosulfate standard titration solution consumed in the titration, ml. V.-the volume of sodium thiosulfate standard titration solution consumed in the blank test, mL; (1)
0.0636---—the mass of steel in grams equivalent to 1.00 ml of sodium thiosulfate standard titration solution Cc(NazSz0,)=1.000 mol/1];
HG/T 2827—1997
C-the actual concentration of sodium thiosulfate standard titration solution, mol/L; m
the mass of the sample·g.
The cuprous cyanide content X2 expressed as a mass percentage is calculated according to formula (2): X = 0. 089 6×(V/-V) ×100
Wherein: V
The volume of sodium thiosulfate standard titration solution consumed in titration, mL; The volume of sodium thiosulfate standard titration solution consumed in blank test, mL; (2)
The mass of cuprous cyanide in grams equivalent to 1.00mL sodium thiosulfate standard titration solution (c(Na2S,O,)=1.000mol/L):
The actual concentration of sodium thiosulfate standard titration solution, mol/L; The mass of the sample, g.
5.3.5 Allowable difference
The arithmetic mean of the parallel determination results is taken as the determination result. The absolute difference (in terms of Cu) of the parallel determination results shall not exceed 0.2%. 5.4 Determination of cyanide (CN) content 5.4.1 Method Summary
The sample is dissolved in an excess of sodium cyanide solution, and the free rat root is titrated with a standard silver nitrate solution. Another blank is made, and the cyanide content can be calculated from the difference in the silver nitrate consumed by the two. 5.4.2 Reagents and Materials
5.4.2.1 Sodium cyanide solution: 40g/L, add 10g of sodium hydroxide per liter; 5.4.2.2 Potassium iodide solution: 10g/L;
5.4.2.3 Standard silver nitrate solution: c(AgNO,) is about 0.1 mol/L. 5.4.3 Analysis Steps
Pipette 10mL of sodium cyanide solution separately, place in 2 conical flasks, weigh about 0.25g of sample (accurate to 0.001g). Place in one of the conical flasks to dissolve. Add 5 mL of potassium iodide solution to each conical flask and titrate with silver nitrate standard titration solution until the turbidity of the solution disappears.
5.4.4 Expression of analysis results
Cyanide content X expressed as mass percentage: calculated according to formula (3): 0.0260 × (V.-V)c × 100
The volume of silver nitrate standard titration solution consumed in titrating the test solution with the sample, mL; V.
--The volume of the standard silver nitrate solution consumed in titrating the test solution without the sample, mL; (3)
0.0260--The mass of cyanide (CN) in grams equivalent to 1.00mL of the standard silver nitrate solution (Cc (AgNO3) = 1.000mol/L);
c---The actual concentration of the standard silver nitrate solution, mol/L, m
The mass of the sample, g.
5.4.5 Allowable difference
The arithmetic mean of the parallel determination results is taken as the determination result. The absolute difference of the parallel determination results shall not exceed 0.2%. 5.5 Determination of insoluble matter in sodium cyanide
5.5.1 Summary of the method
After the sample is dissolved in a certain amount of sodium cyanide solution, it is filtered through glass sand of constant weight, washed with water until the filtrate is neutral, and dried at 105℃~110℃ to constant weight.
5.5.2 Reagents and materials
Sodium cyanide solution: 116g/L.
5.5.3 Instruments and equipment
HG/T 2827—1997
Glass sand crucible: filter plate pore size: 5um~15um. 5.5.4 Analysis steps
Measure 50 ml of sodium cyanide solution, heat it to 50℃±2℃, weigh 5.5 g of sample (accurate to 0.001g), slowly add the sample into the sodium cyanide solution, stir continuously until the sample is completely dissolved, dilute with water to 200 mL: filter with a constant weight glass crucible, wash with water until the filtrate is neutral, and bake the crucible at 105℃～110℃ to constant weight. 5.5.5 Expression of analysis results
The insoluble matter content X in sodium cyanide expressed as mass percentage is calculated according to formula (4): X = ml= mo ×100
Where: mi\
Mass of glass crucible and insoluble matter, m; -Mass of glass crucible, g;
-Mass of sample, g.
5.5.6 Tolerance
Take the arithmetic mean of the parallel determination results as the determination result. The absolute difference between the results of parallel determinations shall not exceed 0.04%. 5.6 Determination of iron content
5.6.1 Summary of the method
Same as Chapter 2 of GB/T3049-1986.
5.6.2 Reagents and materials
Same as Chapter 3 of GB/T3049-1986 and:
5.6.2.1 Nitric acid;
5.6.2.2 Sulfuric acid;
5.6.2.3 Nitrogen water;
5.6.2.4 Sulfuric acid solution: 1+10.
5.6.3 Instruments and equipment
Same as Chapter 4 of GB/T3049--1986.
5.6.4 Analysis steps
5.6.4.1 Drawing of working curve
According to the provisions of 5.3 of GB/T3049-1986, use a 3cm absorption cell and the corresponding amount of iron standard solution to draw the working curve.
5.6.4.2 Preparation of test solution
Weigh about 5 samples (accurate to 0.001g) and place them in a 250mL beaker. Operate in a fume hood, add 8ml nitric acid to moisten the sample, then add 6mL sulfuric acid, stir with a glass rod, and heat until the yellow smoke is exhausted and a large amount of white smoke appears. Cool, add a small amount of water to dissolve, cool to room temperature, add ammonia water until precipitation appears and then dissolve into a dark blue solution, filter with medium-speed filter paper, wash with 100ml warm water with 3ml ammonia water until the filtrate is no longer blue, place the funnel with precipitation on a 500ml volumetric flask, dissolve the precipitation in the funnel with 25ml sulfuric acid solution, wash with warm water several times, dilute to the scale, and shake. 5.6.4.3 Preparation of blank test solution
Except for not adding sample, the rest is the same as the preparation of test solution. 5.6.4.4 Determination
Use a pipette to transfer 20ml of test solution into a 100ml volumetric flask, and operate together with the blank solution according to the provisions of 5.4 of GB/T3049-1986, starting from "add water to about 60ml if necessary". 5.6.4.5 Expression of analysis results
Iron (Fe) content X expressed as mass percentage. Calculate according to formula (5): 703
HG/T2827-1997
X:- (mm)x10
The amount of iron found from the working curve according to the measured absorbance of the test solution, mg; The amount of iron found from the working curve according to the measured absorbance of the blank test solution, mg; m, --
The mass of the sample, g.
5.6.4.6 Allowable difference
The arithmetic mean of the parallel determination results is taken as the determination result. The absolute difference between the two parallel determination results shall not exceed 0.004%. 6 Marking, packaging, transportation, purchase and storage
6.1 The packaging of industrial cuprous cyanide should be firmly and clearly marked, including: manufacturer name, factory address, product name, trademark, grade, net weight, batch number or production date, this standard number and the "highly toxic" mark specified in 13 of GB190-1990. 6.2 Each batch of products leaving the factory should have a quality certificate. The content includes: manufacturer name, factory address, product name, trademark, grade, net weight, batch number or production date, proof that the product quality meets this standard and the number of this standard. 6.3 Industrial cuprous cyanide is packaged in iron drums. Lined with a layer of polyvinyl chloride film bag, the thickness is not less than 0.07mm. The net weight of each drum is 10kg, 15kg, 25kg, 40kg, 50kg. The wall thickness of the iron drum for railway transportation should not be less than 0.80mm. 6.4 The inner bag of the packaging is sealed with two ties or heat seals to ensure a tight seal, and the iron drum cover should be firmly sealed. 6.5T. Industrial cuprous cyanide products should be transported in accordance with the requirements for the transportation of dangerous goods. 6.6I. Industrial cuprous cyanide products must not be mixed with acidic substances and food during storage. 7 Safety requirements
7.1I Industrial cuprous cyanide is a highly toxic substance. During the test, hydrogen cyanide gas may escape, so the test should be conducted in a fume hood. When the cyanide waste liquid generated during the test cannot be returned to production, it shall be handled in accordance with Appendix A of this standard. 7.2 Workers should wear work clothes and protective equipment at the work site, and work clothes and supplies should have a dedicated storage location. 7.3 Product packaging should be destroyed after use and should not be reused. 704
HG/T 2827—1997
Appendix A
(Appendix to the standard)
Treatment of cyanide waste liquid
In order to prevent the pollution of cyanide waste liquid, the waste liquid should be treated before it can be discharged. A1 Method Summary
In an alkaline medium, hypochlorite is used as an oxidant to oxidize cyanide and decompose it into non-toxic nitrogen and carbon dioxide. A2
Treatment steps
Collect the waste liquid in a container of about 10 liters, add 40% sodium hydroxide until the pH value of the waste liquid is greater than 8.5 (check with pH test paper), add bleaching powder in a fume hood and stir thoroughly until the pH value is excessive (check with KI test paper). Leave it for 12 hours before discharging. 705001g). Place in one of the conical flasks to dissolve. Add 5mL of potassium iodide solution to each conical flask and titrate with silver nitrate standard titration solution until the solution becomes turbid and no longer turbid.
5.4.4 Expression of analysis results
Cyanide content X expressed as mass percentage: Calculated according to formula (3): 0.0260 × (V.-V)c × 100
The volume of silver nitrate standard titration solution consumed in titrating the test solution with the sample, mL; V.
--The volume of the standard silver nitrate solution consumed in titrating the test solution without the sample, mL; (3)
0.0260--The mass of cyanide (CN) in grams equivalent to 1.00mL of the standard silver nitrate solution (Cc (AgNO3) = 1.000mol/L);
c---The actual concentration of the standard silver nitrate solution, mol/L, m
The mass of the sample, g.
5.4.5 Allowable difference
The arithmetic mean of the parallel determination results is taken as the determination result. The absolute difference of the parallel determination results shall not exceed 0.2%. 5.5 Determination of insoluble matter in sodium cyanide
5.5.1 Summary of the method
After the sample is dissolved in a certain amount of sodium cyanide solution, it is filtered through glass sand of constant weight, washed with water until the filtrate is neutral, and dried at 105℃~110℃ to constant weight.
5.5.2 Reagents and materials
Sodium cyanide solution: 116g/L.
5.5.3 Instruments and equipment
HG/T 2827—1997
Glass sand crucible: filter plate pore size: 5um~15um. 5.5.4 Analysis steps
Measure 50 ml of sodium cyanide solution, heat it to 50℃±2℃, weigh 5.5 g of sample (accurate to 0.001g), slowly add the sample into the sodium cyanide solution, stir continuously until the sample is completely dissolved, dilute with water to 200 mL: filter with a constant weight glass crucible, wash with water until the filtrate is neutral, and bake the crucible at 105℃～110℃ to constant weight. 5.5.5 Expression of analysis results
The insoluble matter content X in sodium cyanide expressed as mass percentage is calculated according to formula (4): X = ml= mo ×100
Where: mi\
Mass of glass crucible and insoluble matter, m; -Mass of glass crucible, g;
-Mass of sample, g.
5.5.6 Tolerance
Take the arithmetic mean of the parallel determination results as the determination result. The absolute difference between the results of parallel determinations shall not exceed 0.04%. 5.6 Determination of iron content
5.6.1 Summary of the method
Same as Chapter 2 of GB/T3049-1986.
5.6.2 Reagents and materials
Same as Chapter 3 of GB/T3049-1986 and:
5.6.2.1 Nitric acid;
5.6.2.2 Sulfuric acid;
5.6.2.3 Nitrogen water;
5.6.2.4 Sulfuric acid solution: 1+10.
5.6.3 Instruments and equipment
Same as Chapter 4 of GB/T3049--1986.
5.6.4 Analysis steps
5.6.4.1 Drawing of working curve
According to the provisions of 5.3 of GB/T3049-1986, use a 3cm absorption cell and the corresponding amount of iron standard solution to draw the working curve.
5.6.4.2 Preparation of test solution
Weigh about 5 samples (accurate to 0.001g) and place them in a 250mL beaker. Operate in a fume hood, add 8ml nitric acid to moisten the sample, then add 6mL sulfuric acid, stir with a glass rod, and heat until the yellow smoke is exhausted and a large amount of white smoke appears. Cool, add a small amount of water to dissolve, cool to room temperature, add ammonia water until precipitation appears and then dissolve into a dark blue solution, filter with medium-speed filter paper, wash with 100ml warm water with 3ml ammonia water until the filtrate has no blue color, place the funnel with precipitation on a 500ml volumetric flask, dissolve the precipitation in the funnel with 25ml sulfuric acid solution, wash with warm water several times, dilute to the scale, and shake. 5.6.4.3 Preparation of blank test solution
Except for not adding sample, the rest is the same as the preparation of test solution. 5.6.4.4 Determination
Use a pipette to transfer 20ml of test solution into a 100ml volumetric flask, and operate together with the blank solution according to the provisions of 5.4 of GB/T3049-1986, starting from "add water to about 60ml if necessary". 5.6.4.5 Expression of analysis results
Iron (Fe) content X expressed as mass percentage. Calculate according to formula (5): 703
HG/T2827-1997
X:- (mm)x10
The amount of iron extracted from the working curve according to the measured absorbance of the test solution, mg; The amount of iron extracted from the working curve according to the measured absorbance of the blank test solution, mg; m, --
The mass of the sample, g.
5.6.4.6 Allowable difference
The arithmetic mean of the parallel determination results is taken as the determination result. The absolute difference between the two parallel determination results shall not exceed 0.004%. 6 Marking, packaging, transportation, purchase and storage
6.1 The packaging of industrial cuprous cyanide should be firmly and clearly marked, including: manufacturer name, factory address, product name, trademark, grade, net weight, batch number or production date, this standard number and the "highly toxic" mark specified in 13 of GB190-1990. 6.2 Each batch of products leaving the factory should have a quality certificate. The content includes: manufacturer name, factory address, product name, trademark, grade, net weight, batch number or production date, proof that the product quality meets this standard and the number of this standard. 6.3 Industrial cuprous cyanide is packaged in iron drums. Lined with a layer of polyvinyl chloride film bag, the thickness is not less than 0.07mm. The net weight of each drum is 10kg, 15kg, 25kg, 40kg, 50kg. The wall thickness of the iron drum for railway transportation should not be less than 0.80mm. 6.4 The inner bag of the packaging is sealed with two ties or heat seals to ensure a tight seal, and the iron drum cover should be firmly sealed. 6.5T. Industrial cuprous cyanide products should be transported in accordance with the requirements for the transportation of dangerous goods. 6.6I. Industrial cuprous cyanide products must not be mixed with acidic substances and food during storage. 7 Safety requirements
7.1I Industrial cuprous cyanide is a highly toxic substance. During the test, hydrogen cyanide gas may escape, so the test should be conducted in a fume hood. When the cyanide waste liquid generated during the test cannot be returned to production, it shall be handled in accordance with Appendix A of this standard. 7.2 Workers should wear work clothes and protective equipment at the work site, and work clothes and supplies should have a dedicated storage location. 7.3 Product packaging should be destroyed after use and should not be reused. 704
HG/T 2827—1997
Appendix A
(Appendix to the standard)
Treatment of cyanide waste liquid
In order to prevent the pollution of cyanide waste liquid, the waste liquid should be treated before it can be discharged. A1 Method Summary
In an alkaline medium, hypochlorite is used as an oxidant to oxidize cyanide and decompose it into non-toxic nitrogen and carbon dioxide. A2
Treatment steps
Collect the waste liquid in a container of about 10I, add 40% sodium hydroxide until the pH value of the waste liquid is greater than 8.5 (check with pH test paper), add bleaching powder in a fume hood and stir thoroughly until the pH value is excessive (check with KI test paper). Leave it for 12 hours before discharging. 705001g). Place in one of the conical flasks to dissolve. Add 5mL of potassium iodide solution to each conical flask and titrate with silver nitrate standard titration solution until the solution becomes turbid and no longer turbid.
5.4.4 Expression of analysis results
Cyanide content X expressed as mass percentage: Calculated according to formula (3): 0.0260 × (V.-V)c × 100
The volume of silver nitrate standard titration solution consumed by titrating the test solution with the sample, mL; V.
-The volume of the standard silver nitrate solution consumed in titrating the test solution without the sample, mL; (3)
0.0260-The mass of cyanide (CN) in grams equivalent to 1.00mL of the standard silver nitrate solution (Cc (AgNO3) = 1.000mol/L);
c——-The actual concentration of the standard silver nitrate solution, mol/L, m
The mass of the sample, g.
5.4.5 Allowable difference
The arithmetic mean of the parallel determination results is taken as the determination result. The absolute difference of the parallel determination results shall not exceed 0.2%. 5.5 Determination of insoluble matter in sodium cyanide
5.5.1 Summary of the method
After the sample is dissolved in a certain amount of sodium cyanide solution, it is filtered through glass sand of constant weight, washed with water until the filtrate is neutral, and dried at 105℃~110℃ to constant weight.
5.5.2 Reagents and materials
Sodium cyanide solution: 116g/L.
5.5.3 Instruments and equipment
HG/T 2827—1997
Glass sand crucible: filter plate pore size: 5um~15um. 5.5.4 Analysis steps
Measure 50 ml of sodium cyanide solution, heat it to 50℃±2℃, weigh 5.5 g of sample (accurate to 0.001g), slowly add the sample into the sodium cyanide solution, stir continuously until the sample is completely dissolved, dilute with water to 200 mL: filter with a constant weight glass crucible, wash with water until the filtrate is neutral, and bake the crucible at 105℃～110℃ to constant weight. 5.5.5 Expression of analysis results
The insoluble matter content X in sodium cyanide expressed as mass percentage is calculated according to formula (4): X = ml= mo ×100
Where: mi\
Mass of glass crucible and insoluble matter, m; -Mass of glass crucible, g;
-Mass of sample, g.
5.5.6 Tolerance
Take the arithmetic mean of the parallel determination results as the determination result. The absolute difference between the results of parallel determinations shall not exceed 0.04%. 5.6 Determination of iron content
5.6.1 Summary of the method
Same as Chapter 2 of GB/T3049-1986.
5.6.2 Reagents and materials
Same as Chapter 3 of GB/T3049-1986 and:
5.6.2.1 Nitric acid;
5.6.2.2 Sulfuric acid;
5.6.2.3 Nitrogen water;
5.6.2.4 Sulfuric acid solution: 1+10.
5.6.3 Instruments and equipment
Same as Chapter 4 of GB/T3049--1986.
5.6.4 Analysis steps
5.6.4.1 Drawing of working curvewwW.bzxz.Net
According to the provisions of 5.3 of GB/T3049-1986, use a 3cm absorption cell and the corresponding amount of iron standard solution to draw the working curve.
5.6.4.2 Preparation of test solution
Weigh about 5 samples (accurate to 0.001g) and place them in a 250mL beaker. Operate in a fume hood, add 8ml nitric acid to moisten the sample, then add 6mL sulfuric acid, stir with a glass rod, and heat until the yellow smoke is exhausted and a large amount of white smoke appears. Cool, add a small amount of water to dissolve, cool to room temperature, add ammonia water until precipitation appears and then dissolve into a dark blue solution, filter with medium-speed filter paper, wash with 100ml warm water with 3ml ammonia water until the filtrate has no blue color, place the funnel with precipitation on a 500ml volumetric flask, dissolve the precipitation in the funnel with 25ml sulfuric acid solution, wash with warm water several times, dilute to the scale, and shake. 5.6.4.3 Preparation of blank test solution
Except for not adding sample, the rest is the same as the preparation of test solution. 5.6.4.4 Determination
Use a pipette to transfer 20ml of test solution into a 100ml volumetric flask, and operate together with the blank solution according to the provisions of 5.4 of GB/T3049-1986, starting from "add water to about 60ml if necessary". 5.6.4.5 Expression of analysis results
Iron (Fe) content X expressed as mass percentage. Calculate according to formula (5): 703
HG/T2827-1997
X:- (mm)x10
The amount of iron extracted from the working curve according to the measured absorbance of the test solution, mg; The amount of iron extracted from the working curve according to the measured absorbance of the blank test solution, mg; m, --
The mass of the sample, g.
5.6.4.6 Allowable difference
The arithmetic mean of the parallel determination results is taken as the determination result. The absolute difference between the two parallel determination results shall not exceed 0.004%. 6 Marking, packaging, transportation, purchase and storage
6.1 The packaging of industrial cuprous cyanide should be firmly and clearly marked, including: manufacturer name, factory address, product name, trademark, grade, net weight, batch number or production date, this standard number and the "highly toxic" mark specified in 13 of GB190-1990. 6.2 Each batch of products leaving the factory should have a quality certificate. The content includes: manufacturer name, factory address, product name, trademark, grade, net weight, batch number or production date, proof that the product quality meets this standard and the number of this standard. 6.3 Industrial cuprous cyanide is packaged in iron drums. Lined with a layer of polyvinyl chloride film bag, the thickness is not less than 0.07mm. The net weight of each drum is 10kg, 15kg, 25kg, 40kg, 50kg. The wall thickness of the iron drum for railway transportation should not be less than 0.80mm. 6.4 The inner bag of the packaging is sealed with two ties or heat seals to ensure a tight seal, and the iron drum cover should be firmly sealed. 6.5T. Industrial cuprous cyanide products should be transported in accordance with the requirements for the transportation of dangerous goods. 6.6I. Industrial cuprous cyanide products must not be mixed with acidic substances and food during storage. 7 Safety requirements
7.1I Industrial cuprous cyanide is a highly toxic substance. During the test, hydrogen cyanide gas may escape, so the test should be conducted in a fume hood. When the cyanide waste liquid generated during the test cannot be returned to production, it shall be handled in accordance with Appendix A of this standard. 7.2 Workers should wear work clothes and protective equipment at the work site, and work clothes and supplies should have a dedicated storage location. 7.3 Product packaging should be destroyed after use and should not be reused. 704
HG/T 2827—1997
Appendix A
(Appendix to the standard)
Treatment of cyanide waste liquid
In order to prevent the pollution of cyanide waste liquid, the waste liquid should be treated before it can be discharged. A1 Method Summary
In an alkaline medium, hypochlorite is used as an oxidant to oxidize cyanide and decompose it into non-toxic nitrogen and carbon dioxide. A2
Treatment steps
Collect the waste liquid in a container of about 10 liters, add 40% sodium hydroxide until the pH value of the waste liquid is greater than 8.5 (check with pH test paper), add bleaching powder in a fume hood and stir thoroughly until the pH value is excessive (check with KI test paper). Leave it for 12 hours before discharging. 7053 Apparatus and equipment
HG/T 2827—1997
Glass sand crucible: filter plate pore size: 5um~15um. 5.5.4 Analysis steps
Measure 50ml sodium cyanide solution, heat to 50℃±2℃, weigh 5.5g sample (accurate to 0.001g), slowly add the sample to the sodium cyanide solution, stir continuously until the sample is completely dissolved, dilute with water to 200mL: filter with a constant weight glass crucible, wash with water until the filtrate is neutral, and bake the crucible at 105℃~110℃ to constant weight. 5.5.5 Expression of analysis results
The insoluble matter content X in sodium cyanide expressed as mass percentage is calculated according to formula (4): X = ml = mo × 100
Wherein: ml
Mass of glass crucible and insoluble matter, m; -Mass of glass crucible, g;
Mass of sample, g.
5.5.6 Allowable difference
The arithmetic mean of the parallel determination results is taken as the determination result. The absolute difference of the parallel determination results shall not exceed 0.04%. 5.6 Determination of iron content
5.6.1 Summary of method
Same as Chapter 2 of GB/T3049-1986.
5.6.2 Reagents and materials
Same as Chapter 3 of GB/T3049-1986 and:
5.6.2.1 Nitric acid;
5.6.2.2 Sulfuric acid;
5.6.2.3 Nitrogen water;
5.6.2.4 Sulfuric acid solution: 1+10.
5.6.3 Instruments and equipment
Same as Chapter 4 of GB/T3049--1986.
5.6.4 Analysis steps
5.6.4.1 Drawing of working curve
Draw the working curve using a 3 cm absorption cell and the corresponding amount of iron standard solution according to the provisions of 5.3 of GB/T3049-1986.
5.6.4.2 Preparation of test solution
Weigh about 5 samples (accurate to 0.001g) and place them in a 250mL beaker. Perform the operation in a fume hood, add 8ml nitric acid to moisten the sample, then add 6mL sulfuric acid, stir with a glass rod, and heat until the yellow smoke is exhausted and a large amount of white smoke appears. Let it cool, add a small amount of water to dissolve, cool to room temperature, add ammonia water until a precipitate appears and then dissolves into a dark blue solution, filter with medium-speed filter paper, wash with 100ml warm water with 3ml ammonia water until the filtrate has no blue color, place the funnel with the precipitate on a 500ml volumetric flask, dissolve the precipitate in the funnel with 25mL sulfuric acid solution, wash with warm water several times, dilute to the scale, and shake the hook. 5.6.4.3 Preparation of blank test solution
Except for not adding the sample, the rest is the same as the preparation of the test solution. 5.6.4.4 Determination
Use a pipette to transfer 20 ml of the test solution into a 100 ml volumetric flask, and together with the blank solution, proceed from "add water to about 60 ml if necessary" according to the provisions of 5.4 of GB/T3049-1986. 5.6.4.5 Expression of analysis results
The iron (Fe) content X expressed as a mass percentage. Calculate according to formula (5): 703
HG/T2827-1997
X:- (mm)x10
The amount of iron found from the working curve according to the measured absorbance of the test solution, mg; The amount of iron found from the working curve according to the measured absorbance of the blank test solution, mg; m, --
The mass of the sample, g.
5.6.4.6 Tolerance
Take the arithmetic mean of the results of the parallel determinations as the determination result. The absolute difference between the results of two parallel determinations shall not exceed 0.004%. 6 Marking, packaging, transportation, purchase and storage
6.1 The packaging of industrial cuprous cyanide shall be firmly and clearly marked, including: manufacturer name, factory address, product name, trademark, grade, net weight, batch number or production date, this standard promotion number and the "highly toxic" mark specified in 13 of GB190-1990. 6.2 Each batch of products leaving the factory shall have a quality certificate. The content includes: manufacturer name, factory address, product name, trademark, grade, net weight, batch number or production date, proof that the product quality complies with this standard and this standard number. 6.3 Industrial cuprous cyanide is packaged in iron drums. Lined with a layer of polyvinyl chloride film bag, the thickness is not less than 0.07mm. The net weight of each drum is 10kg, 15kg, 25kg, 40kg, 50kg. The wall thickness of the iron drum for railway transportation should not be less than 0.80mm. 6.4 The inner bag of the package shall be sealed with two ties or heat seals to ensure a tight seal, and the iron drum cover shall be firmly sealed. 6.5T. Industrial cuprous cyanide products shall be transported in accordance with the requirements for the transportation of dangerous goods. 6.6I. Industrial cuprous cyanide products shall not be mixed with acidic substances and food during storage. 7 Safety requirements
7.1I Industrial cuprous cyanide is a highly toxic substance. Hydrogen cyanide gas may escape during the test, and the test should be carried out in a ventilated kitchen. When the cyanide waste liquid generated during the test cannot be returned to production, it shall be handled in accordance with Appendix A of this standard. 7.2 Workers should wear work clothes and protective equipment at the work site, and work clothes and supplies should have a special storage place. 7.3 Product packaging should be destroyed after use and shall not be used again. 704
HG/T 2827—1997
Appendix A
(Appendix to the standard)
Treatment of cyanide-containing waste liquid
In order to prevent the pollution of cyanide-containing waste liquid, the waste liquid should be treated before discharge. A1 Method Summary
In an alkaline medium, hypochlorite is used as an oxidant to oxidize and decompose cyanide into non-toxic nitrogen and carbon dioxide. A2
Treatment steps
Collect the waste liquid in a container of about 10I., add 40% sodium hydroxide until the pH value of the waste liquid is greater than 8.5 (check with pH test paper), add bleaching powder in a fume hood and stir thoroughly until it is excessive (check with KI test paper). Let it stand for 12 hours before discharge. 7053 Apparatus and equipment
HG/T 2827—1997
Glass sand crucible: filter plate pore size: 5um~15um. 5.5.4 Analysis steps
Measure 50ml sodium cyanide solution, heat to 50℃±2℃, weigh 5.5g sample (accurate to 0.001g), slowly add the sample to the sodium cyanide solution, stir continuously until the sample is completely dissolved, dilute with water to 200mL: filter with a constant weight glass crucible, wash with water until the filtrate is neutral, and bake the crucible at 105℃~110℃ to constant weight. 5.5.5 Expression of analysis results
The insoluble matter content X in sodium cyanide expressed as mass percentage is calculated according to formula (4): X = ml = mo × 100
Wherein: ml
Mass of glass crucible and insoluble matter, m; -Mass of glass crucible, g;
Mass of sample, g.
5.5.6 Allowable difference
The arithmetic mean of the parallel determination results is taken as the determination result. The absolute difference of the parallel determination results shall not exceed 0.04%. 5.6 Determination of iron content
5.6.1 Summary of method
Same as Chapter 2 of GB/T3049-1986.
5.6.2 Reagents and materials
Same as Chapter 3 of GB/T3049-1986 and:
5.6.2.1 Nitric acid;
5.6.2.2 Sulfuric acid;
5.6.2.3 Nitrogen water;
5.6.2.4 Sulfuric acid solution: 1+10.
5.6.3 Instruments and equipment
Same as Chapter 4 of GB/T3049--1986.
5.6.4 Analysis steps
5.6.4.1 Drawing of working curve
Draw the working curve using a 3 cm absorption cell and the corresponding amount of iron standard solution according to the provisions of 5.3 of GB/T3049-1986.
5.6.4.2 Preparation of test solution
Weigh about 5 samples (accurate to 0.001g) and place them in a 250mL beaker. Perform the operation in a fume hood, add 8ml nitric acid to moisten the sample, then add 6ml sulfuric acid, stir with a glass rod, and heat until the yellow smoke is completely released and a large amount of white smoke appears. Let it cool, add a small amount of water to dissolve, cool to room temperature, add ammonia water until a precipitate appears and then dissolves into a dark blue solution, filter with medium-speed filter paper, wash with 100ml warm water with 3ml ammonia water until the filtrate has no blue color, place the funnel with the precipitate on a 500ml volumetric flask, dissolve the precipitate in the funnel with 25ml sulfuric acid solution, wash with warm water several times, dilute to the scale, and shake to hook. 5.6.4.3 Preparation of blank test solution
Except for not adding the sample, the rest is the same as the preparation of the test solution. 5.6.4.4 Determination
Use a pipette to transfer 20 ml of the test solution into a 100 ml volumetric flask, and together with the blank solution, proceed with the operation starting from “add water to about 60 ml if necessary” according to the provisions of 5.4 of GB/T3049-1986. 5.6.4.5 Expression of analysis results
The iron (Fe) content X expressed as a mass percentage. Calculate according to formula (5): 703
HG/T2827-1997
X:- (mm)x10
The amount of iron found from the working curve according to the measured absorbance of the test solution, mg; The amount of iron found from the working curve according to the measured absorbance of the blank test solution, mg; m, --
The mass of the sample, g.
5.6.4.6 Tolerance
Take the arithmetic mean of the results of the parallel determinations as the determination result. The absolute difference between the results of two parallel determinations shall not exceed 0.004%. 6 Marking, packaging, transportation, purchase and storage
6.1 The packaging of industrial cuprous cyanide shall be firmly and clearly marked, including: manufacturer name, factory address, product name, trademark, grade, net weight, batch number or production date, this standard promotion number and the "highly toxic" mark specified in 13 of GB190-1990. 6.2 Each batch of products shipped shall have a quality certificate. The content includes: manufacturer name, factory address, product name, trademark, grade, net weight, batch number or production date, proof that the product quality complies with this standard and this standard number. 6.3 Industrial cuprous cyanide is packaged in iron drums. Lined with a layer of polyvinyl chloride film bag, the thickness is not less than 0.07mm. The net weight of each drum is 10kg, 15kg, 25kg, 40kg, 50kg. The wall thickness of the iron drum for railway transportation should not be less than 0.80mm. 6.4 The inner bag of the package shall be sealed with two ties or heat seals to ensure a tight seal, and the iron drum cover shall be firmly sealed. 6.5T. Industrial cuprous cyanide products shall be transported in accordance with the requirements for the transportation of dangerous goods. 6.6I. Industrial cuprous cyanide products shall not be mixed with acidic substances and food during storage. 7 Safety requirements
7.1I Industrial cuprous cyanide is a highly toxic substance. Hydrogen cyanide gas may escape during the test, and the test should be carried out in a ventilated kitchen. When the cyanide waste liquid generated during the test cannot be returned to production, it shall be handled in accordance with Appendix A of this standard. 7.2 Workers should wear work clothes and protective equipment at the work site, and work clothes and supplies should have a special storage place. 7.3 Product packaging should be destroyed after use and shall not be used again. 704
HG/T 2827—1997
Appendix A
(Appendix to the standard)
Treatment of cyanide-containing waste liquid
In order to prevent the pollution of cyanide-containing waste liquid, the waste liquid should be treated before discharge. A1 Method Summary
In an alkaline medium, hypochlorite is used as an oxidant to oxidize and decompose cyanide into non-toxic nitrogen and carbon dioxide. A2
Treatment steps
Collect the waste liquid in a container of about 10I., add 40% sodium hydroxide until the pH value of the waste liquid is greater than 8.5 (check with pH test paper), add bleaching powder in a fume hood and stir thoroughly until it is excessive (check with KI test paper). Let it stand for 12 hours before discharge. 7054, start the operation from "add water to about 60mL if necessary". 5.6.4.5 Expression of analysis results
Iron (Fe) content X expressed as mass percentage. Calculate according to formula (5): 703
HG/T2827-1997
X: - (mm) x10
Iron found from the working curve according to the measured absorbance of the test solution, mg; Iron found from the working curve according to the measured absorbance of the blank test solution, mg; m, --
Mass of the sample, g.
5.6.4.6 Allowable difference
The arithmetic mean of the parallel determination results is taken as the determination result. The absolute difference between the two parallel determination results shall not exceed 0.004%. 6 Marking, packaging, transportation, purchase and storage
6.1 The packaging of industrial cuprous cyanide should be firmly and clearly marked, including: manufacturer name, factory address, product name, trademark, grade, net weight, batch number or production date, this standard promotion number and the "highly toxic" mark specified in 13 of GB190-1990. 6.2 Each batch of products leaving the factory should have a quality certificate. The content includes: manufacturer name, factory address, product name, trademark, grade, net weight, batch number or production date, proof that the product quality meets this standard and this standard number. 6.3 Industrial cuprous cyanide is packaged in iron drums. Lined with a layer of polyvinyl chloride film bag, the thickness is not less than 0.07mm. The net weight of each drum is 10kg, 15kg, 25kg, 40kg, 50kg. The wall thickness of the iron drum for railway transportation should not be less than 0.80mm. 6.4 The inner bag of the packaging is sealed with two ties or heat seals to ensure a tight seal, and the iron drum cover should be sealed firmly. 6.5T. Industrial cuprous cyanide products should be transported in accordance with the requirements for dangerous goods transportation. 6.6I. Industrial cuprous cyanide products should not be stored together with acidic substances and food during storage. 7 Safety requirements
7.1I Industrial cuprous cyanide is a highly toxic substance. Hydrogen cyanide gas may escape during the test, so the test should be carried out in a ventilated kitchen. When the cyanide waste liquid generated during the test cannot be returned to production, it should be treated in accordance with Appendix A of this standard. 7.2 Workers should wear work clothes and protective equipment at the work site, and work clothes and supplies should have a special storage place. 7.3 Product packaging should be destroyed after use and should not be used again. 704
HG/T 2827—1997
Appendix A
(Appendix to the standard)
Treatment of cyanide waste liquid
In order to prevent the pollution of cyanide waste liquid, the waste liquid should be treated before it can be discharged. A1 Method Summary
In alkaline medium, use hypochlorite as oxidant to decompose cyanide into non-toxic nitrogen and carbon dioxide. A2
Processing Steps
Collect the waste liquid in a container of about 10 liters, add 40% sodium hydroxide until the pH value of the waste liquid is greater than 8.5 (check with pH test paper), add bleaching powder in a fume hood and stir thoroughly until the pH value is excessive (check with KI test paper). Leave for 12 hours before discharging. 7054, start the operation from "add water to about 60mL if necessary". 5.6.4.5 Expression of analysis results
Iron (Fe) content X expressed as mass percentage. Calculate according to formula (5): 703
HG/T2827-1997
X: - (mm) x10
Iron found from the working curve according to the measured absorbance of the test solution, mg; Iron found from the working curve according to the measured absorbance of the blank test solution, mg; m, --
Mass of the sample, g.
5.6.4.6 Allowable difference
The arithmetic mean of the parallel determination results is taken as the determination result. The absolute difference between the two parallel determination results shall not exceed 0.004%. 6 Marking, packaging, transportation, purchase and storage
6.1 The packaging of industrial cuprous cyanide should be firmly and clearly marked, including: manufacturer name, factory address, product name, trademark, grade, net weight, batch number or production date, this standard promotion number and the "highly toxic" mark specified in 13 of GB190-1990. 6.2 Each batch of products leaving the factory should have a quality certificate. The content includes: manufacturer name, factory address, product name, trademark, grade, net weight, batch number or production date, proof that the product quality meets this standard and this standard number. 6.3 Industrial cuprous cyanide is packaged in iron drums. Lined with a layer of polyvinyl chloride film bag, the thickness is not less than 0.07mm. The net weight of each drum is 10kg, 15kg, 25kg, 40kg, 50kg. The wall thickness of the iron drum for railway transportation should not be less than 0.80mm. 6.4 The inner bag of the packaging is sealed with two ties or heat seals to ensure a tight seal, and the iron drum cover should be sealed firmly. 6.5T. Industrial cuprous cyanide products should be transported in accordance with the requirements for dangerous goods transportation. 6.6I. Industrial cuprous cyanide products should not be stored together with acidic substances and food during storage. 7 Safety requirements
7.1I Industrial cuprous cyanide is a highly toxic substance. Hydrogen cyanide gas may escape during the test, so the test should be carried out in a ventilated kitchen. When the cyanide waste liquid generated during the test cannot be returned to production, it should be treated in accordance with Appendix A of this standard. 7.2 Workers should wear work clothes and protective equipment at the work site, and work clothes and supplies should have a special storage place. 7.3 Product packaging should be destroyed after use and should not be reused. 704
HG/T 2827—1997
Appendix A
(Appendix to the standard)
Treatment of cyanide waste liquid
In order to prevent the pollution of cyanide waste liquid, the waste liquid should be treated before it can be discharged. A1 Method Summary
In alkaline medium, use hypochlorite as oxidant to decompose cyanide into non-toxic nitrogen and carbon dioxide. A2
Processing Steps
Collect the waste liquid in a container of about 10 liters, add 40% sodium hydroxide until the pH value of the waste liquid is greater than 8.5 (check with pH test paper), add bleaching powder in a fume hood and stir thoroughly until the pH value is excessive (check with KI test paper). Leave for 12 hours before discharging. 705
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