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GB 27585-2011: [GB/T 27585-2011] Potassium cyanide for industrial use
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Basic data

Standard ID	GB 27585-2011 (GB27585-2011)
Description (Translated English)	[GB/T 27585-2011] Potassium cyanide for industrial use
Sector / Industry	National Standard
Classification of Chinese Standard	G12
Classification of International Standard	71.060.50
Word Count Estimation	14,167
Date of Issue	2011-12-05
Date of Implementation	2012-08-01
Quoted Standard	GB 190-2009; GB/T 191-2008; GB/T 6678; GB/T 6680; GB/T 6682-2008; GB/T 8170; GB 19268-2003; HG/T 3696.1; HG/T 3696.2; HG/T 3696.3
Regulation (derived from)	Announcement of Newly Approved National Standards No. 19 of 2011
Issuing agency(ies)	General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China, Standardization Administration of the People's Republic of China
Summary	This Chinese standard specifies the requirements for industrial potassium cyanide, test methods, inspection rules, marking, labeling, packaging, transportation, storage, and security requirements. This standard applies to industrial solid potassium cyanide and potassium cyanide solution industry. The products are mainly used in chemical, electroplating, metallurgy and mineral processing industries.

GB 27585-2011: [GB/T 27585-2011] Potassium cyanide for industrial use

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Potassium cyanide for industrial use ICS 71.060.50 G12 National Standards of People's Republic of China Industrial potassium cyanide Issued on. 2011-12-05 2012-08-01 implementation Administration of Quality Supervision, Inspection and Quarantine of People's Republic of China Standardization Administration of China released

Foreword

All the technical contents of this standard is mandatory. This standard is to modify the use of Russian Standard ΓΟСТ8465. 1979 (1988) "Industrial potassium cyanide technical conditions." Taking into account China's national conditions, in the use of Russian Standard ΓΟСТ8465. 1979 (1988), the present standard do some modifications. For technical Differences have been incorporated into the body and they are involved in terms of the margin of a single vertical line identification. Is given in Appendix A and Appendix B List of the technical differences, structural differences and the reasons for the reference. This standard Annex A, Annex B and Annex C is informative appendix. The standard proposed by China Petroleum and Chemical Industry Association. This standard by the National Standardization Technical Committee chemical inorganic chemicals Club (SAC/TC63/SC1) centralized. This standard was drafted. Anqing Shuguang Chemical Co., Ltd., CNOOC Tianjin Chemical Research & Design Institute. Drafters of this standard. Yu Wing, Guofeng Xin, Chen Zhangbin, Wang Lin, Zhang Jingjuan. Industrial potassium cyanide

1 Scope

This standard specifies requirements for industrial potassium cyanide, test methods, inspection rules, marking, labeling, packaging, transportation, storage, and security requirements. This standard applies to industrial solid potassium cyanide and potassium cyanide solution industry. The products are mainly used in chemical, electroplating, metallurgy and mineral processing industries.

2 Normative references

The following documents contain provisions which, through reference in this standard and become the standard terms. For dated references, subsequent Amendments (not including errata content) or revisions do not apply to this standard. However, encourage the parties to the agreement Research on whether to use the latest versions of these documents. For undated reference documents, the latest versions apply to this standard. GB 190-2009 dangerous goods packaging logo GB/T 191-2008 Packaging - Pictorial signs (ISO 780.1997, MOD) GB/T 6678 General Principles for Sampling Chemical Products GB/T 6680 General rules for sampling liquid chemical products GB/T 6682-2008 analytical laboratory use specifications and test methods (ISO 3696. 1987, MOD) GB/T 8170 repair value expressed about the rules and limit values and judgment GB 19268-2003 Packaging solid cyanide Preparation of standard titration solution of HG/T 3696.1 inorganic chemical products, chemical analysis Preparation of HG/T 3696.2 inorganic chemical products, chemical analysis of impurity standard solution Preparations of HG/T 3696.3 inorganic chemical products, chemical analysis

3 formula and relative molecular mass

Molecular formula. KCN Molecular Weight. 65.12 (according to 2007 international relative atomic mass)

4 Requirements

4.1 Appearance. industrial solid potassium should be white flake, lumpy or crystalline particles; industrial potassium cyanide solution should be colorless or light yellow transparent solution. 4.2 Industrial potassium cyanide should meet the requirements of Table 1. Table 1 Requirements project index solid Premium grade First grade Solution Potassium cyanide (KCN), w /% ≥ 99.0 98.5 30.0 Potassium hydroxide (KOH), w /% ≤ 0.3 0.4 1.6 Potassium carbonate (K2CO3), w /% ≤ 0.3 0.5 1.6 Potassium (HCOOK), w /% ≤ 0.9 - - Chloride (Cl dollars), w /% ≤ 0.1 0.2 - Water, w /% ≤ 0.3 0.5 - Water-insoluble, w /% ≤ 0.05 0.05 -

5 Test methods

5.1 Security Warnings Potassium cyanide is virulent, in the sampling and analysis operations should be strictly in accordance with the standard safety requirements. See Appendix analysis of waste C methods for processing. Analysis of the acid, alkali and other corrosive agents, users should be careful to avoid splashing on the skin. As splashed skin On skin, wash immediately with plenty of water, severe cases should be treated immediately. 5.2 General Provisions The standard reagents and water, did not indicate when additional requirements are specified analytical reagent refers to 6682-2008 and GB/T 's Three water. Standard titration solution used in the tests, the impurity standard solution, preparations and products, did not indicate when the other requirements, according HG/T 3696.1, the provisions prepared HG/T 3696.2 and HG/T 3696.3 of. 5.3 appearance of discrimination Under natural light conditions, with visual discrimination method. 5.4 Determination of potassium content 5.4.1 Silver nitrate method (Arbitration Act) 5.4.1.1 Method summary Ammonia medium, silver ions form a complex with cyanide ion, potassium iodide and excess silver ions form a yellow precipitate, indicating the endpoint of the titration. Potassium content is calculated according to consumption and the concentration of the standard silver nitrate titration solution. 5.4.1.2 Reagents 5.4.1.2.1 ammonia solution. 23; 5.4.1.2.2 standard silver nitrate titration solution. c (AgNO3) about 0.05mol/L; 5.4.1.2.3 potassium iodide solution indicates. 50g/L; 5.4.1.2.4 carbon dioxide-free water. 5.4.1.3 Preparation of test solution Weigh 3g ~ 3.5g or 9g ~ 10g solid sample liquid sample, accurate to 0.0002g, dissolved carbon dioxide-free water. then Transferred to 500mL volumetric flask, diluted with carbon dioxide-free water to the mark. This solution was used as test solution A, containing potassium cyanide for The amount determined potassium content, potassium content, potassium content and chloride content. 5.4.1.4 analysis step Pipette with a pipette 25mL of test solution A, placed in a conical flask, add 75mL water, 1mL 1mL aqueous ammonia solution and potassium iodide solution Solution, titration with standard silver nitrate titration Lawrence turbidity of the end. 5.4.1.5 Calculation Results Potassium content of potassium cyanide (KCN) mass fraction w1 and its value is expressed in%, according to equation (1). w1 = (V/1000) cM m (25/500) × 100 (1) Where. Numerical V --- volume of the standard silver nitrate titration solution consumed in titration, in milliliters (mL); C --- accurate standard silver nitrate titration solution concentration value in units of moles per liter (mol/L); Numerical m --- sample mass, in grams (g); Numerical molar mass of the M --- potassium cyanide (2KCN), in units of grams per mole (g/mol) (M = 130.24). Take the arithmetic mean of the parallel determination results of the measurement results, the results of two parallel determination of the absolute difference is not more than 0.3%. 5.4.2 Method of nickel nitrate 5.4.2.1 Method summary Ammonia medium, nickel ions form a complex with cyanide ion, nickel ion and excess diacetyldioxime generate bright red flocculent precipitate means It shows the titration end point. According to the consumption of nickel nitrate titration solution and the standard silver nitrate titration solution conversion factors and standard silver nitrate titration solution Concentration solution of potassium cyanide content was calculated. 5.4.2.2 Reagents and materials 5.4.2.2.1 ammonia solution. 23; 5.4.2.2.2 potassium iodide solution. 50g/L; 5.4.2.2.3 standard silver nitrate titration solution. c (AgNO3) about 0.05mol/L; 5.4.2.2.4 nickel nitrate titration solution. Preparation. Weigh 7.27g of nickel nitrate, accurate to 0.01g, was dissolved in 1000mL of water, shake. Calibration solution of nickel nitrate titration conversion factor standard silver nitrate titration solution (K). Using a pipette, take 25mL test solution A (5.4.1.3), placed in a conical flask, add 75mL of water and 6-8 drops of dimethylglyoxime solution, titration with a nickel nitrate solution was titrated to bright red flocculation Like precipitation occurred so far; then pipette Pipette 25mL test solution A (5.4.1.3), placed in another conical flask, add 75mL water, 1mL 1mL ammonia and potassium iodide solution, titration with standard silver nitrate titration Lawrence turbidity as the end point. Take three parallel determination results used to calculate the arithmetic mean of the conversion factor (K) values. Three replicates poor no more than 0.04mL. Nickel nitrate titration solution to the conversion factor standard silver nitrate titration solution K, according to equation (2). K = V2V1 (2) Where. V1 --- three measured values of nickel nitrate titration solution volume average consumption in milliliters (mL); Value V2 --- three times to determine the average consumption of the standard silver nitrate titration solution volume in milliliters (mL). The results should be expressed to four decimal places. 5.4.2.2.5 diacetyldioxime ammonia solution. 5g/L. 5.4.2.3 analysis step Pipette Pipette 25mL test solution A (5.4.1.3), placed in a conical flask, add 75mL of water and 6-8 drops of ammonia Diacetyldioxime Solution, a solution of nickel nitrate titration titration end point appears under a bright red flocculent precipitate when the solution turned bright yellow, constantly shaking. 5.4.2.4 Calculation Results Potassium content of potassium cyanide (KCN) mass fraction w1 and its value is expressed in%, according to equation (3) Calculated. w1 = (V/1000) cMK m (25/500) × 100 (3) Where. Numerical solution of nickel nitrate titration volume V --- titration consumption in milliliters (mL); C --- accurate standard silver nitrate titration solution concentration value in units of moles per liter (mol/L); K --- nickel nitrate titration solution exact value of the conversion factor standard silver nitrate titration solution of; Numerical m --- sample quality according to 5.4.1.3 weighed in grams (g); Numerical molar mass of the M --- potassium cyanide (2KCN), in units of grams per mole (g/mol) (M = 130.24). Take the arithmetic mean of the parallel determination results of the measurement results, the results of two parallel determination of the absolute difference is not more than 0.3%. 5.5 Determination of potassium content 5.5.1 Method summary Masking solution of nickel nitrate titration of cyanide ions with carbonate ions with barium chloride, using phenolphthalein as the indicator solution, titration with standard hydrochloric acid solution Titrated potassium hydroxide, potassium hydroxide content is calculated according to consumption and the concentration of hydrochloric acid standard titration solution. 5.5.2 Reagents 5.5.2.1 barium chloride solution. 100g/L; 5.5.2.2 hydrochloric acid standard titration solution. c (HCl) approximately 0.02mol/L; Pipette Pipette 20mL press HG/T 3696.1 formulated c (HCl) approximately 1mol/L hydrochloric acid standard titration solution, placed 1000mL volumetric flask, dilute to the mark, shake. 5.5.2.3 phenolphthalein indicator solution. 10g/L; 5.5.2.4 carbon dioxide-free water. 5.5.3 Instruments Microburette. indexing is 0.02mL. 5.5.4 Analysis of step Pipette with a pipette 25mL of test solution A (5.4.1.3), placed in a conical flask, 50mL of carbon dioxide-free water was added and The same volume of nickel nitrate titration solution consumed during titration of 5.4.2.3, and then excess 0.1mL ~ 0.2mL, strong shaking. Join Barium chloride solution 10mL, shake well placed after 1min ~ 2min 15min. Add 2 drops of phenolphthalein indicator solution, titration with hydrochloric acid standard solution Titration to the red disappears. 5.5.5 Calculation Results Potassium content of potassium hydroxide (KOH) mass fraction w2 and its value is expressed in%, according to equation (4) Calculated. w2 = (V/1000) cM m (25/500) × 100 (4) Where. Numerical V --- hydrochloric acid standard titration solution volume consumed by titration, in milliliters (mL); Accurate c --- hydrochloric acid standard titration solution concentration value in units of moles per liter (mol/L); Numerical m --- sample quality according to 5.4.1.3 weighed in grams (g); --- The M values of the molar mass of potassium hydroxide (KOH), in units of grams per mole (g/mol) (M = 56.10). Take the arithmetic mean of the parallel determination results of the measurement results, the results of two parallel determination of the absolute difference is not more than 0.05%. 5.6 Determination of potassium carbonate 5.6.1 Method summary Nickel nitrate solution was titrated with masking cyanide ions, phenolphthalein as an indicator solution, titration with hydrochloric acid standard solution titration total alkali content, minus hydroxide Potassium content. 5.6.2 Reagents 5.6.2.1 hydrochloric acid standard titration solution. with 5.5.2.2; 5.6.2.2 phenolphthalein indicator solution. 10g/L; 5.6.2.3 carbon dioxide-free water. 5.6.3 Instruments Microburette. indexing is 0.02mL. 5.6.4 Analysis of step Pipette with a pipette 25mL of test solution A (5.4.1.3), placed in a conical flask, 50mL of carbon dioxide-free water was added and Nickel nitrate standard titration solution of the same volume consumed during titration 5.4.2.3, then excess 0.1mL ~ 0.2mL, strong shaking. Join 2 drops of phenolphthalein indicator solution, titration with hydrochloric acid standard titration solution to the red disappears. 5.6.5 Calculation Results Potassium content of potassium carbonate (K2CO3) mass fraction w3 and its value is expressed in%, according to equation (5) Calculated. w3 = [(V-V0)/1000] cM m (25/500) × 100 (5) Where. V --- titration consumption hydrochloric acid standard titration solution volume value in milliliters (mL); V0 --- 5.5.5 by titration consumption hydrochloric acid standard titration solution volume value in milliliters (mL); Accurate c --- hydrochloric acid standard titration solution concentration value in units of moles per liter (mol/L); Numerical m --- sample quality according to 5.4.1.3 weighed in grams (g); Numerical molar mass of the M --- potassium carbonate (K2CO3), in units of grams per mole (g/mol) (M = 138.20). Take the arithmetic mean of the parallel determination results of the measurement results, the results of two parallel determination of the absolute difference is not more than 0.05%. 5.7 Determination of potassium content 5.7.1 Principle of the method The use of silver ions and cyanide ions generated silver cyanide precipitation of cyanide to eliminate interference. Under strong basic conditions with potassium permanganate Anti It should, generated in the reaction and excess potassium permanganate under acidic conditions to react with potassium iodide. With sodium thiosulfate and the resulting anti-iodine Should, in order to determine the indirect iodometry potassium content, reaction is as follows. Ag CN- = AgCN ↓ 2MnO4- HCOO- 3OH- = 2MnO42- CO32- 2H2O MnO42- 4I- 8H = Mn2 2I2 4H2O 2MnO4- 10I- 16H = 2Mn2 5I2 8H2O I2 2S2O32- = S4O62- 2I- 5.7.2 Reagents 5.7.2.1 potassium iodide; 5.7.2.2 sodium hydroxide solution. 100g/L; 5.7.2.3 sulfuric acid solution. 19; 5.7.2.4 silver nitrate solution. 17g/L; 5.7.2.5 potassium permanganate solution. c 15KMnO ÷ 4 about 0.1mol/L; 5.7.2.6 sodium thiosulfate standard titration solution. c (Na2S2O3) about 0.1mol/L; 5.7.2.7 phenolphthalein indicator solution. 10g/L; 5.7.2.8 Starch indicator solution. 5g/L. 5.7.3 Analysis of step Pipette with a pipette 50mL of test solution A (5.4.1.3), placed in 250mL conical flask, add 1mL of sodium hydroxide was added dropwise Silver nitrate solution, plus side shaking, until brown precipitated. With rapid qualitative filter paper, the precipitate was washed with water until the filtrate was not Alkaline (test solution with phenolphthalein indicator). The filtrate and washings were collected in 250mL iodine bottle, add 2mL sodium hydroxide solution is added accurately 25mL potassium permanganate solution, heated in boiling water for 20min, then cool to room temperature. Add 2g of potassium iodide, and then quickly added 10mL sulfur Acid solution, shake stamped, seal, placed in the dark for 5min. Standard titration with sodium thiosulfate solution titration, was added near the end 2mL lake Pink indicator solution and continue titration to the disappearance of the blue solution as the end point. Make a blank test simultaneously. Blank test. in addition to omission of sample addition, the type and amount of addition of reagents and other operations with the same sample solution. 5.7.4 Calculation Results Potassium content of potassium (HCOOK) mass fraction w4 and its value is expressed in%, according to equation (6) Calculated. w4 = [(V0-V)/1000] cM m (50/500) × 100 (6) Where. Blank test value V0 --- sodium thiosulfate standard titration solution volume consumed in milliliters (mL); Numerical V --- sodium thiosulfate standard titration titration solution volume consumed in milliliters (mL); Accurate c --- sodium thiosulfate standard titration solution concentration value in units of moles per liter (mol/L); Numerical m --- sample quality according to 5.4.1.3 weighed in grams (g); M --- potassium 12 Numerical ÷ HCOOK molar mass in grams per mole (g/mol) (M = 42.06). Take the arithmetic mean of the parallel determination results of the measurement results, the results of two parallel determination of the absolute difference is not more than 0.1%. 5.8 Determination of chloride content 5.8.1 Method summary Acid and heating the sample to eliminate interference potassium cyanide, and then add silver nitrate solution, turbidity and chloride standard solution produced by the resulting Turbidity comparison. 5.8.2 Reagents 5.8.2.1 nitric acid solution. 19. 5.8.2.2 silver nitrate solution. 17g/L. 5.8.2.3 glacial acetic acid. 11. 5.8.2.4 Chloride Standard solution. 1mL solution of chlorine (Cl) 0.1mg; Preparation. Pipette Pipette 10mL chloride standard solution according to HG/T 3696.2 prepared, placed in 100mL flask with water Dilute to the mark. 5.8.2.5 hydrogen cyanide detection test. if desired, the filter paper strip was immersed in an equal volume ratio of a solution prepared solution was mixed with the solution prepared in 2 Preparation of test strips. Solution 1 and solution preparation method is as follows. Solution 1. about 1g/L of o-tolidine acetate solution of 0.64g --- the o-tolidine 5mL dissolved in glacial acetic acid, with Diluted with water to 1L. Solution 2. 1g/L copper acetate solution. 5.8.3 Instruments Colorimetric tube. 50mL 5.8.4 Analysis of step Warning. This operation was conducted exhaust ventilation hood. Pipette with a pipette 5mL of sample solution A (5.4.1.3), placed in 150mL beaker. Add 50mL water, placed in a fume hood, add 6mL nitric acid solution, cover the surface of the dish, boil until the test with no hydrogen cyanide hydrogen cyanide detection test date (no blue color). Cooled, Rinse surface water dish, the solution was transferred to a colorimetric tube, dilute with water to volume, and mix. Take six colorimetric tubes, each added 45mL of water, 5mL nitric acid solution. Were added 0mL, 0.20mL, 0.40mL, 0.60mL, 0.80mL and 1.00mL chloride standard solution, and shake. In each added colorimetric tube 1mL silver nitrate solution, mix the sample solution and standard solution with a black background will be compared. 5.8.5 Calculation Results Chloride content quality chlorine (Cl) scores w5 and its value is expressed in%, according to equation (7) Calculated. w5 = m1 m (5/500) × 100 (7) Where. m1 --- and turbidity samples corresponding to the standard colorimetric tube mass values of chlorine, in milligrams (mg); m --- Press (5.4.1.3) weighed sample mass value in grams (g). Take the arithmetic mean of the parallel determination results of the measurement results, the results of two parallel determination of the absolute difference is not more than 0.03%. 5.9 Determination of Moisture 5.9.1 instruments and equipment 5.9.1.1 weighing bottle. φ45mm × 25mm; 5.9.1.2 electric oven. the temperature can be controlled at 105 ℃ ~ 110 ℃. 5.9.2 Analysis of step Previously used at 105 ℃ ~ 110 ℃ drying to constant mass weighing bottle weighed 3g ~ 5g solid sample, accurate to 0.0002g. Moved into the electric oven, open the lid, at 105 ℃ ~ 110 ℃ drying 2.5h. Removed, placed in a desiccator, cooled 30min. Weighing, accurate to 0.0002g. 5.9.3 Calculation Results Moisture mass fraction w6 and its value is expressed in%, according to equation (8) Calculated. w6 = m1-m2m × 100 (8) Where. Value m1 --- dried before weighing bottle and the sample mass, in grams (g); m2 --- dried numerical weighing bottle and the sample mass, expressed in grams (g); Numerical m --- sample mass, in grams (g). Take the arithmetic mean of the parallel determination results of the measurement results, the results of two parallel determination of the absolute difference is not more than 0.03%. 5.10 Determination of water-insoluble matter content 5.10.1 Reagent Silver nitrate solution. 50g/L. 5.10.2 instruments and equipment 5.10.2.1 sintered glass crucible. filter plate pore size of 5μm ~ 15μm; 5.10.2.2 electric oven. the temperature can be controlled at 105 ℃ ~ 110 ℃. 5.10.3 analysis step Weigh about 5g of solid samples, accurate to 0.01g, beaker, add 10mL ~ 12mL of hot water (50 ℃ ~ 60 ℃) was dissolved. use Previously dried to a constant mass of glass sand filtration crucible at 105 ℃ ~ 110 ℃, washed with hot water until the filtrate was free from cyanide ion (with Solution of silver nitrate test). The glass sand crucible together with insolubles be transferred to the electric oven at 105 ℃ ~ 110 ℃ drying to Constant quality. The filtrate was treated in accordance with Appendix C. 5.10.4 Calculation Results Water-insoluble mass fraction w7 and its value is expressed in%, according to equation (9) Calculated. w7 = m1-m2m × 100 (9) Where. M1 --- sintered glass crucible together insolubles mass value in grams (G); Numerical m2 --- glass crucible sand mass in grams (g); Numerical m --- sample mass, in grams (g). Take the arithmetic mean of the parallel determination results of the measurement results, the results of two parallel determination of the absolute difference is not more than 0.01%.

6 Inspection rules

6.1 uses standard type test and factory inspection. 6.1.1 Table 1, all the project type test project, under normal production conditions, at least every three months a type test. Have When one of the following circumstances, it should be type tested. a) Replace the key production process; b) The main raw material change; c) to resume production after a shutdown; d) factory inspection results are quite different and the last type test. 6.1.2 Table 1 potassium content, potassium content, potassium content, chloride content, potassium content, water factory inspection items Currently, batches should be tested. 6.2 Solid potassium cyanide. the company with the same material, the same basic production conditions, continuous production or yield daily batch; potassium cyanide dissolved Each batch of liquid product does not exceed 60t. 6.3 solid potassium cyanide determine the sampling units according to the provisions of GB/T 6678's. Sampling, the sampler from the top of the drums to feed Xiecha Layer 3/4 of the sampling depth. Bulk sampling and sheet products, after first removing the upper 15cm layer of material sampled from each of the selected package The sample was taken less than 50g. The samples will be mined by mixing with sample splitter or by quartering reduced to less than 100g. Potassium cyanide solution according to the provisions of GB T 6680/sampling, sampling from the discharge port storage tanks, tankers, and sample volume of not less than 100mL. The recovery of the sample aliquots in two clean and dry plastic bottle with a ground stopper or jar, sealed. Attach a label on the bottle indicating. Production plant name, product name, grade, batch number, date of sampling and sampling by name. As a laboratory sample bottle, another bottle for future reference, like potassium cyanide Product shelf life of more than 15d. 6.4 manufacturer shall ensure that each batch of potassium cyanide in line with the industrial requirements of this standard. 6.5 If an indicator test results do not meet the requirements of this standard should be twice the amount of packaging from re-sampling retest, retest results that is So that only an indicator does not meet the requirements of this standard, then the entire batch of products falling grades or failed. 6.6 using GB/T 8170 provisions of rounding value comparison tes...

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