Wednesday, June 22, 2011

ANALYSIS METHOD OF POTASSIUM HUMATE

Currently there is no National standard, Trade standard in China for Humate series products, so we compile this Enterprise Standard to ensure the steady production. This standard is compiled according to the GB/T1.1-2000< The structure of Standard and the Rules of Compile> stipulated in the first part of .

Analysis of Potassium Humate

a./ Application range
This standard is used for the Humic acid analysis in Potassium Humate that is made from lignite and weathering coal, etc.

b./ Quality Demand
The quality must meet up with the following standards:
Analysis items Standards
A B
Humic acid(dry basis) 80%min 65%min
Moisture 15%max 15%max
Potassium Oxide 7.5%min 10-12%
Ph value of 1% solution 9-10 9-10

c./ Analysis method (Gravimetric method)

.analyze contents of total Humic acid

1. test facilities and instruments
a./ tropical drying box with temperature controlled at 110±5℃.
b./ centrifuge with rotate speed at least 2000r/min and its volume above 150ml.
c./ tropical water bath
d./ muffle roaster
e./ filter paper.
f./ weighing bottle with ground-glass stopper; diameter 500mm, height 30mm.

2. Reagents and solutions
a./ Sodium Pyrophosphate(HGB-1288)chemically pure
b./ Sodium Hydrate(GB629-81) chemically pure
c./ Alkaline extraction solvent of Sodium Pyrophosphate
Weigh 15g Sodium Pyrophosphate and 7g Sodium Hydrate and then dissolve them into l liter distilled water and keep at airproof place.

3. Process of analysis

a./ dissolve
weigh 0.2g sample(precision 0.0002g) and put into 250ml conical flask, then add 100.00ml Alkaline extraction solvent of Sodium Pyrophosphate,shake it to make sure the sample is wet. Insert glass-filler an put them into boiling water bath, heat and extract for 2hours and shake it in every 30miuntes during this time.

b./ Centrifugation
take out the flask, cool to room temperature(about 20℃), then put whole extraction liquid and residue into centrifugal glass and centrifugalize it for 30minutes at the speed of 2000r/min. .

c./ filtration
put in advance the filter paper and weighing bottle into 105-110℃ drying box and make them constant weight. Pour away the topper clear liquid by inclining the glass, then transfer the whole residue onto constant-weight filter paper, syringe it till the ph value becomes neutral.

d./ drying
put residue together with filter paper into constant-weight weighing bottle and put them into drying box for 2hours under 105-110℃. Take out, covering and cooling for 3minutes; put again into drying box and cool it to around 20℃(about 20minutes) and weigh it; Make inspective drying and weigh in every 30minutes. Stop doing so till the difference of close analysis weight is within 0.001g, weigh the residue(G1).

e./ignition
Move dried residue and filter paper into crucible and then put into muffle roaster with an aperture of 15-20mm, heat from 20℃ to 250-300℃ to slowly ash this product; close the furnace door, ignite it under 815+/-20℃ for 1 hour; take out in the air for 5 minutes and then put into drying box and cool it to about 20℃(around 20minutes), weigh the ash in the residue(G2).

4. Results calculation
The total content of Humic Acid(HA) is expressed by weight percentage(%) and calculated by following formula:
HA’t. ad = (G-G1+G2) ÷ G x 100 – (Mad+Aad)
Remark : G—the sample weight, g
G1 — Weight of residue, g
G2 — Ash weight, g
Mad — moisture in sample, %
Aad — Ash in sample, %

5. Allowable deviation

HA’t, % Same lab Different lab
ad % d%
<50 1.0 2.0
≥50 2.0 3.0

6. Attention matters
a./ be careful during transferring the extraction residue and first syringe to avoid filter paper-perforation.
b./ to keep the same water volume and syringe times during filtration.
c./ the temperature must be lower 200 while the residue start to become partly into ash, so that the filter paper keeps away from fired.

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