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GB 6549-2011: [GB/T 6549-2011] Potassium chloride
Status: Valid
GB 6549: Historical versions
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[GB/T 6549-2011] Potassium chloride
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| GB 6549-1996 | 439 |
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Potassium chloride
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| GB 6549.1-1986 | 199 |
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Potassium chloride--Determination of potassium content--Potassium tetraphenylborate gravimetric method
| Obsolete |
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Potassium chloride
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Basic data
Standard ID: GB 6549-2011 (GB6549-2011)
Description (Translated English): [GB/T 6549-2011] Potassium chloride
Sector / Industry: National Standard
Classification of Chinese Standard: G12
Classification of International Standard: 71.060.50
Word Count Estimation: 13,166
Date of Issue: 2011-07-20
Date of Implementation: 2012-06-01
Older Standard (superseded by this standard): GB 6549-1996
Quoted Standard: GB/T 6678-2003; GB/T 6679-2003; GB/T 6682; GB/T 8170; GB 8569; GB/T 9723; GB 18382; HG/T 2843
Regulation (derived from): Announcement of Newly Approved National Standards No. 10 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 potassium chloride product classification, requirements, test methods, inspection rules, packaging, labeling, transportation and storage. This standard applies to all kinds of potassium and potassium salt brine produced by a variety of processes and agricultural products with potassium chloride.
GB 6549-2011: [GB/T 6549-2011] Potassium chloride
---This is a DRAFT version for illustration, not a final translation. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.) will be manually/carefully translated upon your order.
Potassium chloride
ICS 71.060.50
G12
National Standards of People's Republic of China
Replacing GB 6549-1996
Potassium chloride
Issued on. 2011-07-20
2012-06-01 implementation
Administration of Quality Supervision, Inspection and Quarantine of People's Republic of China
Standardization Administration of China released
Foreword
The standard Chapter 4, 4.1, 4.2 Table 1 hydroxide and water projects, Chapter 6, Chapter 7, 7.1 and 7.2 are mandatory, which
It was recommended.
This standard replaces GB 6549-1996 "potassium chloride."
This standard compared with GB 6549-1996 The main changes are as follows.
--- Standard scope changed to "applicable to the various types of potassium and potassium salt brine produced in various industrial and agricultural processes chloride
Potassium products ";
--- Simplifies product categories are divided into class Ⅰ and class Ⅱ industrial potassium chloride with potassium chloride agriculture;
--- Modified potassium indicators Class Ⅱ agricultural quality products from the previous version of the standard ≥54% ≥55.0% modified to use;
--- Revised moisture index, with three levels of class Ⅰ industrial water ≤2% from the previous version of the standard, ≤4%, ≤6%, revised to all
≤2.0%; Ⅱ class agricultural three grades from the previous version of the standard all ≤6%, revised to ≤2.0%, ≤4.0%, ≤6.0%;
--- Modify the determination of potassium content, eliminating the step of adding formaldehyde; sodium tetraphenylborate precipitating agent by the addition of 65g/L
10mL changed to 30g/L12mL; potassium tetraphenylborate precipitated detergent from saturated solution of potassium tetraphenylborate changed to 1g/L tetracene
Sodium boron solution.
The standard proposed by China Petroleum and Chemical Industry Association.
This standard is under the jurisdiction of Chemical Industry Standardization Technical Committee chemical mine.
This standard was drafted. even in the blue sea and Design Institute, Sinochem Fertilizer Co., Ltd., SDIC Xinjiang Lop Nur Potash Co., Ltd., China Agricultural
Industry production company, Haixi Aviation tripotassium Silicon Co., Ltd., Qinghai Hanhai Group Limited, Qinghai Oriental quality potassium chloride industry
Pilot plant, Qinghai Potash Corp. Hamachi, Qaidam Mineral Chemical Co., Ltd.
The main drafters of this standard. the king of peace, Zhang Xiaomei, Li Xue word, Feng Mingwei, He Yongfeng, discipline, Li Can first, Quan - yi, Gezhao Min, He Maoxiong,
Cuikui Min.
The standard standard replaces the previous editions.
--- GB 6549-1986;
--- GB 6549-1996.
Potassium chloride
1 Scope
This standard specifies the potassium chloride product classifications, requirements, test methods, inspection rules, packaging, labeling, transportation and storage.
This standard applies to all types of potassium from the potassium salt and brine in various agricultural and industrial production process with potassium chloride products.
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 are based on research
Whether the latest versions of these documents. For undated reference documents, the latest versions apply to this standard.
GB/T 6678-2003 General Principles for Sampling Chemical Products
GB/T 6679-2003 General rules for sampling solid chemical products
GB/T 6682 analytical laboratory use specifications and test methods (GB/T 6682-2008, ISO 3696. 1987, MOD)
GB/T 8170 repair value expressed about the rules and limit values and judgment
GB 8569 solid chemical fertilizers Packaging
GB/T 9723 Chemicals flame atomic absorption spectrometry General
GB 18382 fertilizer identify the content and requirements (GB 18382-2001, neqISO 7409. 1984)
HG/T 2843 fertilizer products for chemical analysis commonly used standard titration solution, standard solution, reagent solution and indicator solution
3 Product Categories
Potassium chloride product use is divided into two categories.
Class Ⅰ for industrial use potassium chloride, used in chemical industry, production of a variety of potash, but also for the preparation of fertilizer or used directly as fertilizer
Administration.
Ⅱ class agricultural potassium chloride, for the preparation of directly as fertilizer or fertilizer application.
4 Requirements
4.1 appearance of white, gray, reddish, light brown powder, granular or crystalline.
4.2 KCl industrial and agricultural products should comply with the technical requirements in Table 1.
Table 1 technical requirements of industrial and agricultural use potassium chloride
project
index
Ⅰ Class Ⅱ Class
Premium grade First grade Qualified Excellence in goods First grade Qualified
Potassium oxide (K2O) mass fraction /% ≥ 62.0 60.0 58.0 60.0 57.0 55.0
Water (H2O) mass fraction /% ≤ 2.0 2.0 2.0 2.0 4.0 6.0
Combined amount of calcium and magnesium (Ca Mg) mass fraction /% ≤ 0.3 0.5 1.2 - - -
Sodium chloride (NaCl) mass fraction /% ≤ 1.2 2.0 4.0 - - -
The mass fraction of water insoluble /% ≤ 0.1 0.3 0.5 - - -
Note 1. In addition to water, the mass fraction of the components are on a dry basis.
Note 2. Ⅰ class combined amount of calcium and magnesium, sodium chloride and water insoluble mass fraction of KCl recommended as an industrial index, agricultural unlimited.
5 Test methods
This standard reagents and water in the absence of other specified requirements, refer to analytical reagent and in line with GB/T 6682 in the three water regulation
grid. The solution in the absence of marked preparation method, according to HG/T 2843 regulations formulated.
5.1 Determination of potassium oxide content of potassium tetraphenylborate gravimetric method
5.1.1 Method summary
After the sample was dissolved in water, heating under alkaline conditions to eliminate interference in a sample of ammonium ions, added disodium edetate eliminate interference points
Analysis of the results of other cations. Potassium and sodium tetraphenylborate reaction of potassium tetraphenylborate precipitate was filtered, dried and weighed.
5.1.2 Reagents and solutions
5.1.2.1 sodium hydroxide solution.200g/L.
5.1.2.2 disodium ethylenediaminetetraacetate (EDTA) solution. 40g/L.
5.1.2.3 sodium tetraphenylborate solution. 30g/L. Weigh 30g of sodium tetraphenylborate [NaB (C6H5) 4], was dissolved in 980mL of water, add 4mL hydrogen
Sodium hydroxide solution, 20mL magnesium chloride solution (100g/LMgCl2 · 6H2O), stirred for 15min, filtered before use.
5.1.2.4 sodium tetraphenylborate washing solution. 1g/L. Filtrate with 30g/L of sodium tetraphenylborate solution formulated by 130.
5.1.2.5 phenolphthalein indicator solution. 5g/L. 0.5g phenolphthalein dissolved in 100mL of ethanol.
5.1.3 Instruments
5.1.3.1 Glass filter crucible. the 4th, 25mL or 30mL.
5.1.3.2 oven. adjustable at 120 ℃ ± 2 ℃.
5.1.4 Analysis of step
5.1.4.1 Preparation of test solution
Weigh about 5g sample, to the nearest 0.001g, placed in 250mL beaker, add 100mL of water, stirring constantly heated micro-boiling
5min, removed, cooled to room temperature and transferred to 500mL volumetric flask, dilute to the mark, shake. This is the solution A.
Dry solution was filtered A, a small amount of initial filtrate was discarded, the filtrate Pipette 25.0mL in 250mL volumetric flask, dilute to the mark, shake
uniform. This is the solution B.
5.1.4.2 Determination
Pipette 50.0mL of solution B in 250mL beaker, 10mLEDTA solution, 2 to 3 drops of phenolphthalein indicator solution, with stirring
Sodium hydroxide solution was added dropwise to an excess of red appeared and 1mL. Heating boil 5min, a solution remains red, volume remains 50mL
about.
Remove the beaker with a little water to wash the cup wall. Under constant stirring, slowly dropped 12mL sodium tetraphenylborate solution and continue stirring 1min, in
Water rapidly cooled to room temperature, placed 10min.
Previously used 120 ℃ drying to constant weight of glass suction filter crucible. First suction supernatant with sodium tetraphenylborate was washed with dumping
The precipitate was washed slope method 4 to 5 times the precipitate to the filter and transferred until the transfer complete precipitation continued for 3 to 4 times with washing liquid in the filter,
Each wash was about 5mL use. Finally, the precipitate was washed with water twice, each time with water to about 5mL.
The precipitate containing filter placed in an oven at 120 ℃ drying 90min. Removed, placed in a desiccator to cool to room temperature, and weighed.
5.1.5 Calculation Results
Potassium oxide (K2O) content w1 mass fraction (%) expressed by the formula (1).
w1 = m1 × 0.1314m × 25/500 × 50/250 × 100 ×
100-w2
= M1 × 1314m ×
100-w2
(1)
Where.
m1 --- potassium tetraphenylborate precipitate mass value in grams (g);
Numerical m --- sample mass, in grams (g);
w2 --- in a sample of water mass fraction,%;
.1314 --- Tetraphenylboron quality potassium hydroxide in terms of the value of the quality factor.
Calculation result to two decimal places, take the arithmetic mean of the parallel determination results for the final determination.
5.1.6 allowable difference
Parallel determination results of the absolute difference should be less than 0.38%.
5.2 Determination of Moisture
5.2.1 Method summary
Sample at 105 ℃ ± 2 ℃ oven drying to reduce moisture content is the quality.
5.2.2 Instruments
5.2.2.1 said vials. with ground glass lid, flat, a diameter of about 60mm, height of about 30mm.
5.2.2.2 oven. adjustable at 105 ℃ ± 2 ℃.
5.2.2.3 dryer. Load the appropriate drying agent, such as discoloration of silica gel.
5.2.3 Analysis of step
Weigh about 5g sample, to the nearest 0.001g, is placed in a pre-dried to a constant weight of 105 ℃ ± 2 ℃ weighing bottle, gently shake weighing
Bottle, so that the sample is uniformly tiled weighing bottle, open weighing bottle, be placed in 105 ℃ ± 2 ℃ oven 120min. Remove say
Flask, capped, into the dryer to cool to room temperature and weighed.
5.2.4 Calculation Results
Water (H2O) content w2 mass fraction (%) expressed by the formula (2).
w2 = m1-m2m × 100
(2)
Where.
m1 --- said vials and sample values before drying mass in grams (g);
m2 --- said vials and sample mass after drying value in units of grams (g);
Numerical m --- sample mass, in grams (g).
Calculation result to two decimal places, take the arithmetic mean of the parallel determination results for the final determination.
5.2.5 allowable difference
When the content is less than or equal to 4.00%, the absolute difference should be less than 0.20%; when the content is more than 4.00%, the absolute difference should be less than
0.30%.
5.3 Determination of calcium and magnesium content
5.3.1 Flame Atomic Absorption Spectrometry
The water test should be consistent with GB/T 6682 in two water specifications.
5.3.1.1 Method summary
Sample was dissolved in water, adding lanthanum chloride eliminate interfering ions, in hydrochloric acid medium, using air - acetylene flame to flame atomic
Absorption spectrometer wavelength absorbance was measured at 422.7nm and 285.2nm to work curve method determined calcium and magnesium.
5.3.1.2 Reagents and solutions
5.3.1.2.1 hydrochloric acid solution. 11.
5.3.1.2.2 KCl. 10g/L.
5.3.1.2.3 lanthanum chloride solution. 100g/L.
5.3.1.2.4 calcium standard solution. 1.00mg/mL. Weigh 2.4972g advance at 105 ℃ ~ 110 ℃ drying 1h and placed in the dryer
Cooled to room temperature and calcium carbonate (purity reagents), placed in 250mL beaker, add 20mL water, hydrochloric acid solution was added dropwise until complete dissolution,
Excess 10mL. Heated to boiling, to make carbon dioxide flooding, remove the cooled to room temperature and transferred to 1000mL volumetric flask, dilute to the mark with water, shake
uniform. The solution calcium (Ca) concentration of 1.00mg/mL.
5.3.1.2.5 calcium standard solution. 100μg/mL. Pipette 100.0mL calcium standard solution (5.3.1.2.4) in 1000mL volumetric flask
Diluted with water to the mark. The solution calcium (Ca) concentration of 100μg/mL.
5.3.1.2.6 Magnesium standard solution. 1.00mg/mL. Weigh 1.6583g previously burned 1h at 900 ℃ and placed in the dryer to cool to
Room temperature magnesium oxide (high purity reagents), placed in 250mL beaker, add 20mL water, 10mL hydrochloric acid solution, micro-heat until completely dissolved. cool down
To room temperature and transferred to 1000mL volumetric flask, dilute to the mark, shake. This solution was magnesium (Mg) concentration of 1.00mg/mL.
5.3.1.2.7 Magnesium Standard solution. 50μg/mL. Pipette 50.0mL magnesium standard solution (5.3.1.2.6) in 1000mL volumetric flask,
Diluted with water to the mark. This solution was magnesium (Mg) concentration of 50μg/mL.
5.3.1.3 Instruments
Flame atomic absorption spectrometer. shall comply with GB/T 9723's.
5.3.1.4 analysis step
5.3.1.4.1 Preparation of the test solution
Table 2 Sample Weigh, to the nearest 0.001g, placed in 250mL beaker, add 100mL water, stirring constantly heated micro-boiling
5min, remove the cooled to room temperature and transferred to 250mL volumetric flask, dilute to the mark with water, shake dry filter, this is the test solution C.
Table 2 above test solution was pipetted C in 100mL volumetric flask, was added a solution of lanthanum chloride 10mL, 4mL dilute hydrochloric acid solution, washed with water
Release to the mark. Blank test solution prepared simultaneously.
Table 2 sample weight and volume of the test solutions Pipette
Calcium or magnesium content /% sample weight/g
Pipette Volume/mL
Calcium and magnesium
< 0.1 2 50.0 50.0
2 20.0 10.0 0.1 0.4
> 0.4 ~ 1 1.0 20.0 10.0
5.3.1.4.2 photometry
Flame atomic absorption spectrometer with an air - acetylene flame, zero water, measured in the test solution and the blank at wavelength 422.7nm
Calcium test solution absorbance by subtracting the absorbance of the test solution absorbance of the blank test solution, corresponding calcium isolated from the working curve
Numerical mass concentration; measuring test solution and the blank test solution of magnesium absorbance at a wavelength at 285.2nm, with the test solution absorbance
Subtract the absorbance of the blank test solution, check out the value of the corresponding concentration of magnesium from the working curve.
5.3.1.4.3 Draw the curve
Pipette respectively 0.0mL, 1.0mL, 2.0mL, 4.0mL, 6.0mL, 8.0mL calcium standard solution (5.3.1.2.5) and magnesium standard solution
Solution (5.3.1.2.7), correspondence, placed in a 100mL flask, add 10mL potassium chloride solution, lanthanum chloride solution and 10mL
4mL dilute hydrochloric acid solution, washed with water to the mark. This series calcium concentration of 0.0μg/mL, 1.0μg/mL, 2.0μg/mL,
4.0μg/mL, 6.0μg/mL, 8.0μg/mL, a magnesium concentration of 0.0μg/mL, 0.5μg/mL, 1.0μg/mL, 2.0μg/mL,
3.0μg/mL, 4.0μg/mL. The absorbance was measured under the same conditions and the absorbance of the test solution and minus zero concentration of the solution, calcium or magnesium
The amount of concentration as abscissa and ordinate corresponding absorbance, drawing working curve.
5.3.1.5 Calculation Results
5.3.1.5.1 calcium (Ca) content w3 mass fraction (%) expressed by the formula (3) Calculated.
w3 = ρ × 100 × 10
-6
m × V/250 × 100 ×
100-w2
(3)
Where.
Value from the working curve ρ --- Richard calcium mass concentration, in micrograms per milliliter (μg/mL);
Numerical m --- sample mass, in grams (g);
V --- Pipette Numerical Test solution volume in milliliters (mL);
w2 --- in a sample of water mass fraction,%.
Calculation result to two decimal places, take the arithmetic mean of the parallel determination results for the final determination.
5.3.1.5.2 magnesium (Mg) content w4 mass fraction (%) expressed by the formula (4) Calculated.
w4 = ρ × 100 × 10
-6
m × V/250 × 100 ×
100-w2
(4)
Where.
Value from the working curve ρ --- Richard magnesium mass concentration, in micrograms per milliliter (μg/mL);
Numerical m --- sample mass, in grams (g);
V --- Pipette Numerical Test solution volume in milliliters (mL);
w2 --- in a sample of water mass fraction,%.
Calculation result to two decimal places, take the arithmetic mean of the parallel determination results for the final determination.
5.3.1.6 allowable difference
When calcium or magnesium content of less than 0.20%, the absolute difference should be less than 0.02%; the content is 0.20% to 1.00%, the absolute difference should be less than
0.04%.
5.3.2 EDTA volumetric method
5.3.2.1 Method summary
Sample was dissolved in water at pH > 12 conditions, the addition of calcium acid indicator, titration with EDTA standard titration solution of calcium; at pH = 10, the
Join chrome black T indicator, titration with EDTA standard solution titration, calcium, magnesium alloy amount to obtain the subtraction magnesium content.
5.3.2.2 Reagents and solutions
5.3.2.2.1 ammonia solution. 11.
5.3.2.2.2 sodium hydroxide solution. 100g/L.
5.3.2.2.3 hydrogen peroxide solution. 110. With 30% hydrogen peroxide formulation.
5.3.2.2.4 triethanolamine solution. 13.
5.3.2.2.5 ammonia - ammonium chloride buffer solution (pH = 10) was weighed 67.5g of ammonium chloride dissolved in water, aqueous ammonia was added 570mL, diluted with water to
1000mL, and mix.
5.3.2.2.6 disodium edetate (EDTA) standard titration solution. c (EDTA) = 0.02mol/L. Preparation and Calibration Press
HG/T 2843 execution.
5.3.2.2.7 calcium acid indicator. Weigh 0.2g of calcium acid indicator [2-hydroxy-1- (2-carboxy-4-sulfonic acid 1-naphthyl) azo-3-naphthoyl
Acid] and 10g of sodium chloride by 110 ℃ dried, placed in a mortar and grind to a fine powder, stored in a brown bottle grinding mouth, into the dryer set aside.
5.3.2.2.8 chrome black T indicator solution. 5g/L. Weigh 0.5g chrome black T, dissolved in 100mL triethanolamine solution (5.3.2.2.4) in.
5.3.2.3 analysis step
5.3.2.3.1 Preparation of the test solution
Table 3. Weigh sample to the nearest 0.001g, placed in 400mL beaker, add 150mL of hot water, stirring add 4 to 5 drops of peroxide
Hydrogen solution, heated to a boil without small bubbles (about 5min), remove the cooled to room temperature and transferred to 200mL volumetric flask, dilute to the mark,
Shake well.
5.3.2.3.2 Determination of calcium content
Table 3 Pipette test solution in 250mL beaker, dilute with water to about 100mL, was added 5mL triethanolamine solution, hydroxide
Sodium solution was adjusted to pH > 12, calcium acid indicator a little, stir well, titration with EDTA standard solution titration to the solution from pure pale burgundy
Blue end.
5.3.2.3.3 Determination of magnesium content
Table 3 Pipette test solution in 250mL beaker, dilute with water to about 100mL, was added 5mL triethanolamine solution, adding 5mL
Ammonia - ammonium chloride buffer solution and 2 drops of chrome black T indicator solution, stir, titration with EDTA standard solution titration to the solution from pale blue-burgundy
Color is the end.
5.3.2.3.4 blank test
Determination of required sample and determination of calcium and magnesium content in the blank test at the same time.
Table 3 sample weight and volume of the test solutions Pipette
Calcium or magnesium content /% sample weight/g Pipette volume/mL
< 0.1 10 50.0
10 20.0 0.1 0.5
> 0.......
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