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GB/T 13885-2017 English PDF (GBT13885-2017)

GB/T 13885-2017 English PDF (GBT13885-2017)

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GB/T 13885-2017: Determination of the contents of calcium, copper, iron, magnesium, manganese, potassium, sodium and zinc in feeds -- Method using atomic absorption spectrometry

This document specifies the method that uses atomic absorption spectrometry to determine the contents of calcium (Ca), copper (Cu), iron (Fe), magnesium (Mg), manganese (Mn), potassium (K), sodium (Na) and zinc (Zn) in feeds. This Standard is applicable to the determination of the contents of calcium (Ca), copper (Cu), iron (Fe), magnesium (Mg), manganese (Mn), potassium (K), sodium (Na) and zinc (Zn) in compound feeds, concentrate feeds, concentrate supplements, additive premixes and feed ingredients. The detection limit of each element content of this method is: K, Na: 500mg/kg; Ca, Mg: 50mg/kg; Cu, Fe, Mn, Zn: 5mg/kg.
GB/T 13885-2017
GB
NATIONAL STANDARD OF THE
PEOPLE REPUBLIC OF CHINA
ICS 65.120
B 46
Replacing GB/T 13885-2003
Determination of the contents of calcium, copper, iron,
magnesium, manganese, potassium, sodium and zinc in feeds
- Method using atomic absorption spectrometry
(ISO 6869:2000, Animal feeding stuffs - Determination of the contents of calcium, copper, iron, magnesium, manganese, potassium, sodium and zinc - Method using atomic absorption spectrometry, MOD)
ISSUED ON: NOVEMBER 01, 2017
IMPLEMENTED ON: MAY 01, 2018
Issued by: General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China;
Standardization Administration of the People's Republic of China.
Table of Contents
Foreword ... 3
1 Scope ... 5
2 Normative references ... 5
3 Principle ... 6
4 Reagents and solutions ... 6
5 Instruments and equipment ... 7
6 Sampling ... 8
7 Preparation of specimens ... 8
8 Analysis steps ... 8
9 Result calculation ... 11
10 Precision ... 12
11 Inspection report ... 13
Annex A (informative) Structural changes of this Standard compared with ISO 6869:2000 ... 14
Annex B (informative) Technical differences between this Standard and ISO 6869:2000 and their reasons ... 15
Annex C (informative) Laboratory determination results ... 16
Bibliography ... 22
Determination of the contents of calcium, copper, iron,
magnesium, manganese, potassium, sodium and zinc in feeds
- Method using atomic absorption spectrometry
1 Scope
This document specifies the method that uses atomic absorption spectrometry to determine the contents of calcium (Ca), copper (Cu), iron (Fe), magnesium (Mg), manganese (Mn), potassium (K), sodium (Na) and zinc (Zn) in feeds.
This Standard is applicable to the determination of the contents of calcium (Ca), copper (Cu), iron (Fe), magnesium (Mg), manganese (Mn), potassium (K), sodium (Na) and zinc (Zn) in compound feeds, concentrate feeds, concentrate supplements, additive premixes and feed ingredients.
The detection limit of each element content of this method is:
K, Na: 500mg/kg;
Ca, Mg: 50mg/kg;
Cu, Fe, Mn, Zn: 5mg/kg.
2 Normative references
The following referenced documents are indispensable for the application of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. GB/T 6682, Water for analytical laboratory use - Specification and test methods (GB/T 6682-2008, ISO 3696:1987, MOD)
GB/T 14699.1, Feeding stuffs - Sampling (GB/T 14699.1-2005, ISO 6497:2002, IDT)
GB/T 20195, Animal feeding stuffs - Preparation of test samples (GB/T 20195-2006, ISO 6498:1998, IDT)
constant. The contents of Cu, Fe, Mn and Zn in this Standard solution are all 20??g/mL. The standard solution shall be prepared on the day of use.
4.9 Standard stock solutions of Ca, K, Mg, Na: Weigh the following reagents into a 1L volumetric flask:
- 1.907g of potassium chloride (KCl);
- 2.028g of magnesium sulfate (MgSO4??7H2O);
- 2.542g of sodium chloride (NaCl).
Weigh 2.497g of calcium carbonate (CaCO3) into the beaker. Add 50mL of hydrochloric acid solution (4.3).
CAUTION: Be careful of the carbon dioxide produced.
Heat on a heating plate for 5min. After cooling, transfer the solution to a volumetric flask containing K, Mg, Na salts. Use hydrochloric acid solution (4.4) to set the volume constant. The contents of Ca, K and Na in this stock solution are all 1mg/mL. The content of Mg is 200??g/mL.
NOTE: Commercially available standard solutions can be used.
4.10 Standard solutions of Ca, K, Mg, Na: Accurately pipette 25.0mL of stock solution (4.9) into a 250mL volumetric flask. Use hydrochloric acid solution (4.4) to set the volume constant. The contents of Ca, K and Na in this standard solution are all 100??g/mL. The content of Mg is 20??g/mL. The prepared standard solutions are stored in polyethylene bottles. They can be used within 1 week.
4.11 Lanthanum/cesium blank solution: Take 5mL of lanthanum nitrate solution, 5mL of cesium chloride solution and 5mL of hydrochloric acid solution (4.3) into a 100mL volumetric flask. Use water to set the volume constant.
5 Instruments and equipment
All containers, including pipettes for preparing standard solutions, are rinsed with hydrochloric acid solution (4.4) before use. If special ashing crucibles and glassware are used, there is no need to boil them with hydrochloric acid solution before each use. Common laboratory equipment and special equipment are as follows.
5.1 Analytical balance: the resolution is 0.1mg.
5.2 Crucible: platinum, quartz or porcelain; free of potassium and sodium; the inner layer is smooth and not corroded; the upper diameter is 4cm~6cm; the lower diameter is 2cm~2.5cm; the height is about 5cm; boil with hydrochloric acid solution (4.3) before use.
5.3 Rigid glassware. Boil with hydrochloric acid solution (4.3) before use. Rinse off with water.
5.4 Heating plate.
5.5 High temperature resistance furnace: the temperature can be controlled at 550?????15???.
5.6 Atomic absorption spectrophotometer: the wavelength range complies with the provisions of 8.6.1 and 8.7.1. It is with air-acetylene flame and background correction. 5.7 Ca, Cu, Fe, K, Mg, Mn, Na, Zn hollow cathode lamps or electrodeless discharge lamps.
5.8 Quantitative filter paper.
6 Sampling
This Standard does not specify the sampling method. It is recommended to sample according to the method in GB/T 14699.1.
It is very important for the laboratory to obtain representative samples. Samples must not be damaged or deteriorated during transportation and storage. The preserved samples shall be protected from deterioration and other changes.
7 Preparation of specimens
Prepare specimens according to GB/T 20195. The crushed particle size of the specimen shall pass through a 0.45mm analytical sieve.
8 Analysis steps
8.1 Check for organic matter
Take some of the test material with a flat spoon. Heat it over a flame. If the test material melts without smoke, there is no organic matter present. If the color of the test material changes and does not melt, the test material contains organic matter.
8.2 Test material
Weigh 1g~5g of test material according to the estimated content, accurate to 1mg. Put it in the crucible. For test material containing organic matter, start from 8.3. For test material not containing organic matter, start directly from 8.4.
solution (4.4) and the absorbance of the standard solution. Subtract the absorbance of the hydrochloric acid solution (4.4) from the absorbance of the standard solution. The calibration curve is plotted against the contents of Cu, Fe, Mn and Zn with the corrected absorbance values.
NOTE 1: Most atomic absorption spectrophotometers have the function of automatically drawing curves.
NOTE 2: Non-linearly drawn curves are not required. If the curve presents a high-order function shape, the method of drawing the curve nonlinearly can improve the accuracy of the measured data. 8.6.3 Determination of test material solution
Under the same conditions, measure the absorbance of the test material solution (8.4) and blank solution (8.5). The absorbance of the test material solution minus the absorbance of the blank solution. Calculate the concentration of elements in the test material solution from the standard curve. Calculate the content according to Chapter 9. If necessary, dilute the sample solution and blank solution with hydrochloric acid solution (4.4). Make its absorbance within the linear range of the standard curve. NOTE 1: Most atomic absorption spectrophotometers have the function of automatically calculating the concentration of elements in the test material solution. NOTE 2: Background correction is not required. If there is a background value, the use of background correction can improve the accuracy of the measured data.
8.7 Determination of calcium, magnesium, potassium, sodium
8.7.1 Measurement conditions
Adjust the instrument test conditions of the atomic absorption spectrophotometer. Make the instrument in the best analysis state in the air-acetylene flame measurement mode. The measuring wavelengths of Ca, K, Mg and Na are as follows:
Ca: 422.6nm;
K: 766.5nm;
Mg: 285.2nm;
Na: 589.6nm.
8.7.2 Standard curve
Use water to dilute to the standard solution (4.10). For every 100mL of standard solution, add 5mL of lanthanum nitrate solution, 5mL of cesium chloride solution and 5mL of hydrochloric acid solution (4.3). Prepare a set of suitable standard working solutions.

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