HG/T 2935-2006 English PDF (HGT2935-2006)

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HG/T 2935-2006: Feed grade ferrous sulfate
HG/T 2935-2006
HG
CHEMICAL INDUSTRY STANDARD
OF THE PEOPLE’S REPUBLIC OF CHINA
ICS 65.120
B 46
Filing No.: 18218-2006
Replacing HG 2935-2000
Feed grade ferrous sulfate
ISSUED ON: JULY 26, 2006
IMPLEMENTED ON: MARCH 01, 2007
Issued by: National Development and Reform Commission of PRC
Table of Contents
Foreword ... 3
1 Scope ... 4
2 Normative references ... 4
3 Categories ... 5
4 Requirements ... 5
5 Test method ... 5
6 Inspection rules ... 16
7 Signs, labels ... 16
8 Packaging, transportation, storage ... 16
Feed grade ferrous sulfate
1 Scope
This standard specifies the requirements, test methods, inspection rules, signs, labels,
packaging, transportation, storage of feed grade ferrous sulfate.
This standard applies to monohydrate or heptahydrate feed grade ferrous sulfate. This
product is used as iron supplement, in feed processing.
Molecular formula: FeSO4 • nH2O, n = 1 or n = 7
Relative molecular mass: 169.92 (n = 1), 278.01 (n = 7) (according to the international
relative atomic mass in 2001)
2 Normative references
The provisions in following documents become the provisions of this Standard through
reference in this Standard. For the dated references, the subsequent amendments
(excluding corrections) or revisions do not apply to this Standard; however, parties who
reach an agreement based on this Standard are encouraged to study if the latest versions
of these documents are applicable. For undated references, the latest edition of the
referenced document applies.
GB/T 1250 Rules for expression and judgement of limiting values
GB/T 6003.1-1997 Test sieves of metal wire cloth
GB/T 6678 General principles for sampling chemical products
GB/T 6682-1992 Water for laboratory use - Specifications (eqv ISO 3696:1987)
GB 10648 Feed label
GB/T 13079-1999 Determination of total arsenic in feeds
GB/T 13080-2004 Determination of lead in feeds - Method using atomic absorption
spectrometry
HG/T 3696.1 Inorganic chemical products - Preparations of standard volumetric
solutions for chemical analysis
HG/T 3696.2 Inorganic chemical products - Preparations of standard solutions for
are required in the test, shall be prepared according to the provisions of HG/T 3696.1,
HG/T 3696.2, HG/T 3696.3.
5.3 Identification test
5.3.1 Reagents
5.3.1.1 Potassium ferricyanide solution: 100 g/L.
5.3.1.2 Barium chloride solution: 50 g/L.
5.3.2 Identification method
5.3.2.1 Identification of sulfate ion
Take a little specimen. Add water to dissolve it. Add barium chloride solution dropwise
to form a white precipitate. This precipitate is insoluble in hydrochloric acid and nitric
acid.
5.3.2.2 Identification of ferrous ions
Take a little specimen. Add water to dissolve it. Add potassium ferricyanide solution
dropwise to form a dark blue precipitate.
5.4 Determination of ferrous sulfate content and iron content
5.4.1 Method summary
After the specimen is dissolved, add sulfur-phosphorus mixed acid. Use sodium
diphenylamine sulfonate as indicator. Use potassium dichromate standard titration
solution for titration to determine the content of ferrous sulfate and iron.
5.4.2 Reagents
5.4.2.1 Thion-phosphorus mixed acid: Add 150 mL of sulfuric acid and 150 mL of
phosphoric acid to 700 mL water. Mix well.
5.4.2.2 Potassium dichromate standard titration solution: c (1/6K2Cr2O7) ≈ 0.05
mol/L.
5.4.2.3 Sodium diphenylamine sulfonate indicator solution: 5 g/L.
5.4.3 Analytical procedures
Weigh about 0.2 g of specimen (accurate to 0.0002 g). Place it in a 250 mL conical flask.
Add 30 mL of water to dissolve it. Add 10 mL of sulfur-phosphorus mixed acid, 2 drops
of sodium diphenylamine sulfonate indicator solution. Immediately use potassium
dichromate standard titration solution to titrate, until the solution turns purple, which is
solution, which is consumed by titrating the blank solution, in milliliters (mL);
c - The exact value of the concentration of potassium dichromate standard titration
solution, in moles per liter (mol/L);
m - The value of sample mass, in grams (g);
M - The molar mass value M (FeSO4 • 7H2O) = 278.0 [or measured by iron (Fe), its
molar mass value M (Fe) = 55.84], when ferrous sulfate heptahydrate product is
measured by ferrous sulfate heptahydrate (FeSO4 • 7H2O), in gram per mole (g/mol).
Take the arithmetic mean value of parallel determination results as measurement result;
the absolute difference of two parallel determination results is not more than 0.3% for
ferrous sulfate; it is not more than 0.1% for the iron content.
5.5 Determination of arsenic content
5.5.1 Silver diethyldithiocarbamate - spectrophotometric method (arbitration
method)
5.5.1.1 Method summary
In acidic medium, arsenic is reduced by zinc to generate arsine gas, then it is introduced
into silver diethyldithiocarbamate [Ag(DDTC)] solution for absorption, so as to form
yellow or brownish red silver sol. The color depth is directly proportional to the content
of arsenic. It is subject to colorimetric determination by a spectrophotometer.
5.5.1.2 Reagents and materials
5.5.1.2.1 Silver diethyldithiocarbamate (Ag-DDTC)-triethylamine-chloroform solution:
2.5 g/L.
5.5.1.2.2 Arsenic standard solution: 1 mL solution contains 50 μg of arsenic (As).
Use a pipette to pipette 5.00 mL of arsenic standard solution, which is prepared
according to HG/T 3696.2. Place it in a 100 mL volumetric flask. Dilute to the mark.
Shake well.
5.5.1.2.3 Arsenic standard solution: 1 mL of solution contains 1 μg of arsenic (As).
Use a pipette to pipette 2.00 mL of arsenic standard solution (5.5.1.2.2), into a 100 mL
volumetric flask. Add 1 mL of hydrochloric acid. Dilute to the mark. Shake well.
Prepare it before use.
5.5.1.2.4 Sulfuric acid solution: 1 + 4.
5.5.1.2.5 Tartaric acid solution: 200 g/L.
5.5.1.2.6 Lead acetate absorbent cotton.
5.5.1.2.7 Potassium iodide solution: 150 g/L.
5.5.1.2.8 Stannous chloride hydrochloric acid solution: Dissolve 40 g of stannous
chloride (SnCl2 • 2H2O) in 50 mL of hydrochloric acid solution (1 + 1). Use water to
dilute it to 100 mL.
5.5.1.2.9 Arsenic-free zinc particles: Particle size (3.0 ± 0.2) mm.
5.5.1.3 Instruments and equipment
Same as Chapter 4 of GB/T 13079-1999.
5.5.1.4 Analytical procedures
5.5.1.4.1 Specimen solution: Weigh about 3 g of specimen, accurate to 0.01 g. Place it
in a 150 mL beaker. Add 10 mL of sulfuric acid solution. Heat it. Slightly boil it for 2
min. After cooling, completely transfer to the arsenic bottle. Add 25 mL of tartaric acid
solution. Shake well. Add water to 40 mL.
5.5.1.4.2 Drawing of working curve: Accurately pipette 0.00 mL, 1.00 mL, 2.00 mL,
4.00 mL, 6.00 mL, 8.00 mL, 10.00 mL of arsenic standard solution, in seven arsenic
generating bottles, respectively. Add 10 mL of sulfuric acid solution each. Add water to
dilute it to 40 mL. Shake well. Measure the absorbance, after operating according to
5.5.1.4.3, to find the regression equation. Draw a standard curve, using the absorbance
as the ordinate and the mass of arsenic (μg) as the abscissa.
5.5.1.4.3 Reduction reaction and colorimetric determination: Add 2 mL of potassium
iodide solution to the specimen solution and working curve solution, respectively.
Shake well. Then add 2 mL of stannous chloride hydrochloric acid solution. Shake well.
Let it stand for 15 min.
Accurately pipette 5.00 mL of Ag-DDTC-triethylamine-chloroform solution, into a dry
ab...