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NY/T 1972-2010 PDF English

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NY/T 1972-2010: Water-soluble fertilizers - Determination of sodium, selenium, silicon content
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NY/T 1972-2010: Water-soluble fertilizers - Determination of sodium, selenium, silicon content

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ICS 65.080 G 20 NY AGRICULTURAL INDUSTRY STANDARD OF THE PEOPLE'S REPUBLIC OF CHINA Water-soluble fertilizers – Determination of sodium, selenium, silicon content Issued on: DECEMBER 23, 2010 Implemented on: FEBRUARY 01, 2011 Issued by. Ministry of Agriculture of the People's Republic of China

Table of Contents

Foreword ... 3 1 Scope ... 4 2 Normative references ... 4 3 Measurement of sodium content ... 4 4 Measurement of selenium content – Atomic fluorescence spectrometric method ... 13 5 Measurement of silicon content - Plasma emission spectrometric method17

Foreword

This standard was drafted in accordance with the provisions of GB/T 1.1-2009. This standard was proposed by AND shall be under the jurisdiction of the Ministry of Agriculture of the People's Republic of China. The drafting organizations of this standard. National Fertilizer Quality Supervision and Inspection Center (Beijing), Ministry of Agriculture - Fertilizer Quality Supervision and Inspection Center (Chengdu), AND Ministry of Agriculture - Fertilizer Quality Supervision and Inspection Center (Ji’nan). The main drafters of this standard. Fan Hongli, Sun Youning, Han Yansong, Liu Mi, Bao Wankui, Song Wenqi, Lu Guiju. Water-soluble fertilizers – Determination of sodium, selenium, silicon content

1 Scope

This standard specifies the test methods for the water-soluble fertilizers – sodium, selenium, AND silicon content measurement. This standard applies to measurement of liquid OR solid water-soluble fertilizers – sodium, selenium, AND silicon content.

2 Normative references

The following documents are essential to the application of this document. For the dated documents, only the versions with the dates indicated are applicable to this document; for the undated documents, only the latest version (including all the amendments) are applicable to this Standard. GB/T 8170 Rules of rounding off for numerical values & expression and judgment of limiting values HG/T 2843 Chemical fertilizer products – Standard volumetric, standard reagent and indicator solutions for chemical analysis NY/T 887 Density testing of liquid fertilizer

3 Measurement of sodium content

3.1 Flame photometric method 3.1.1 Principle The sodium atoms in the sample solution are excited by the thermal energy of the flame; when the excited electron is transited from a higher energy level to a lower energy level, it can release a certain energy, which will generate the spectral line of a fixed wavelength; USE the optical system to measure the radiant energy, in order to obtain the sodium content. 3.1.2 Reagents and materials WEIGH 0.2 g ~ 3 g sample (accurate to 0.0001 g); PLACE it into a 250mL volumetric flask; USE water to make it reach to constant volume; MIX it uniformly; dry FILTER it; DISCARD the first few milliliters of filtrate; USE the rest filtrate for measurement. 3.1.4.3 Drawing of working curve Respectively PIPETTE 0 mL, 1.00 mL, 2.00 mL, 3.00 mL, 4.00 mL, 5.00 mL, 6.00 mL, AND 7.00 mL of sodium standard solution (3.1.2.2) into eight 100 mL volumetric flasks; USE water to make it reach to constant volume; MIX it uniformly. The sodium’s mass concentration of this standard series solution is respectively 0 μg/mL, 1.00 μg/mL, 2.00 μg/mL, 3.00 μg/mL, 4.00 μg/mL, 5.00 μg/mL, 6.00 μg/mL, AND 7.00 μg/mL. On the flame photometer of selected working conditions, based on the sodium concentration of the solution to be tested, SELECT six points from the standard series solution; USE the 0 μg/mL standard solution to adjust the zero point of the instrument; from low concentration to high concentration, respectively MEASURE the emission intensity of each standard solution. USE the sodium’s mass concentration of each standard series solution (μg/mL) as the abscissa AND the corresponding emission intensity as the ordinate; DRAW the working curve. 3.1.4.4 Measurement USE the sample solution OR the solution which is diluted to certain ratio, under the same conditions of the standard series solution for measurement purposes, to measure the emission intensity of sodium; from the working curve, FIND the corresponding mass concentration of the sodium (μg/mL). 3.1.4.5 Blank test Except for not adding of sample, the rest steps are same as the sample solution measurement. 3.1.5. Analysis result presentation The sodium (Na) content w1 is expressed in mass fraction (%), AND calculated in accordance with the equation (1). Where. ρ – The sodium’s mass concentration of the sample solution as found from the working curve, in the unit of micrograms per milliliter (μg/mL); 3.2.2.2 Cesium chloride solution. ρ (CsCl) = 4 g/L. WEIGH 4 g of cesium chloride and DISSOLVE it in water; USE water to dilute it to 1 L; MIX it uniformly. 3.2.2.3 High purity argon. 3.2.3 Instruments 3.2.3.1 Ordinary laboratory instruments; 3.2.3.2 Horizontal reciprocating oscillators OR oscillators with equivalent functions. 3.2.3.3 Plasma emission spectrometer. 3.2.4 Analysis procedures 3.2.4.1 Sample preparation With respect to the solid samples, after multiple times of splitting, TAKE out about 100 g; rapidly GRIND it to the grain which can all pass the 0.50 mm pore size sieve (if the sample is wet, it shall pass through the 1.00 mm pore size sieve); MIX it uniformly; PLACE it in a clean AND dry container; after the liquid sample is subject to multiple times of shaking, quickly TAKE out about 100 mL; PLACE it in a clean AND dry container. 3.2.4.2 Sample solution preparation 3.2.4.2.1 Solid sample WEIGH 0.2 g ~ 3 g of sample (accurate to 0.0001 g); PLACE into a 250 mL volumetric flask; ADD 150 mL of water; PLACE it into the (25 ± 5) °C oscillator; under the oscillating frequency of (180 ± 20) r/min, OSCILLATE it for 30 min; TAKE it out; USE water to make it reach to constant volume; MIX it uniformly; dry FILTER it; DISCARD the first few milliliters of filtrate; USE the rest filtrate for measurement. 3.2.4.2.2 Liquid sample WEIGH 0.2 g ~ 3 g sample (accurate to 0.0001 g); PLACE it into a 250mL volumetric flask; USE water to make it reach to constant volume; MIX it uniformly; dry FILTER it; DISCARD the first few milliliters of filtrate; USE the rest filtrate for measurement. 3.2.4.3 Drawing of working curve 250 – The volume of the sample solution, in the unit of milliliter (mL); m – The mass of the sample, in the unit of grams (g); 106 – The coefficient used to convert g to μg. USE the arithmetic mean of the parallel measurement results as the measurement result, keeping two decimal places. 3.2.6 Allowable difference The relative difference of the parallel measurement results is not more than 10%; The relative difference between the measurement results from different laboratories is not more than 30%. When the measurement result is less than 0.15%, the relative difference of the parallel measurement results AND the measurement results from different laboratories will not be considered. 3.3 Atomic absorption spectrophotometric method 3.3.1 Principle USE the flame emission method of atomic absorption spectrophotometer to measure the sodium content. DO not use the sodium hollow cathode lamp. Under the effect of air – acetylene flame, the sodium in the sample solution is converted into gaseous atom, AND the atom’s outer layer electrons are further excited; when the excited electrons are transited from the higher energy level to the lower energy level, the atom will release the excess energy to produce the spectral line of characteristic emission; within the certain range, the emission spectral line intensity is directly proportional to the sodium atom concentration; through measuring the 330.2 nm emission spectral line intensity, MEASURE the sodium content of the sample. 3.3.2 Reagents and materials The preparation of the reagents, water and solution which are used in this standard shall, unless otherwise indicated of specifications AND preparation methods, be in accordance with the provisions of HG/T 2843. 3.3.2.1 Sodium standard solution. ρ (Na) = 1 mg/mL. 3.3.2.2 Dissolved acetylene. 3.3.3 Instruments concentration range, the fluorescence intensity is directly proportional to the selenium content of the sample solution. 4. 2 Reagents and materials The preparation of the reagents, water and solution which are used in this standard shall, unless otherwise indicated of specifications AND preparation methods, be in accordance with the provisions of HG/T 2843. 4.2.1 Potassium hydroxide solution. ρ (KOH) = 5 g/L. 4.2.2 Potassium borohydride solution. ρ (KBH4) = 20 g/L. WEIGH 10.0 g of potassium borohydride; DISSOLVE it into the 500 mL of potassium hydroxide solution (4. 2.1); MIX it uniformly. 4.2.3 Potassium ferricyanide solution. ρ {K3[Fe(CN)6]} = 20 g/L. 4.2.4 Hydrochloric acid solution. φ (HCl) = 3 %. 4.2.5 Hydrochloric acid solution. φ (HCl) = 50 %. 4.2.6 Selenium standard solution. ρ (Se) = 1000 μg/mL. 4.2.7 Selenium standard solution. ρ (Se) = 10 μg/mL. Accurately PIPETTE 10.00 mL of selenium standard solution (4.2.6); USE hydrochloric acid solution (4.2.4) to make its volume reach to 1000 mL; MIX it ... ......
Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al.


      

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