QUALITY CONTROL

QUALITY CONTROL IN PLANT

Samples are collected on a daily basis, for each lot and run for a granular particle size and moisture. The CEC is typically run on a monthly basis from a composite sample for the month.

 PARTICLE SIZE

Particle size distributions are determined by using a Horiba LA-920 laser scattering particle size distribution analyzer.  Delta Analytical Instruments, Inc. at 1061 Main Street, North Huntington, PA. 15642 (phone 724-864-9850) does the analyses for different speed settings on the variable frequency drive for the whizzer (the classifier). The speed settings produce uniform particle sizes. The 60-cycle setting is what is used for this product. See the attached particle size distribution chart.

GRANULAR PARTICLE SIZES

Granular particle sizes are determined using a rotap with various sample screens. See letter from Ed Huffman dated 28 August 2009

CATION EXCHANGE CAPACITY (CEC)

Representative product samples are collected on a daily basis of all BRZ™. A composite sample is prepared for each month and loaded with nitrogen as follows:

BRZ™ FAST PROCEDURE FOR CEC DETERMINATION, 27 AUGUST 2010

PROCEDURE

• Weigh 100 grams of BRZ™.  Dry sample in drying oven or exactly 2 hours at 100 degrees centigrade.

• Place in a 400 ml. deep beaker

• Just cover the BRZ™ with an ammonium nitrate solution.  Prepare the ammonium nitrate solution by dissolving 20 grams of ammonium nitrate in 15 mls. of  boiling distilled water (this solution is known as “AN 20” in the agricultural world).

• Soak the BRZ™ for 24 hours stirring the beaker at least 2 to 3 times.

• Pour off the ammonium nitrate solution, and let it “drip dry” from the beaker placed on its side.

• Fill the beaker three times as full as the beaker will hold with distilled water and each time stir it with a glass rod, let it soak for one hour, and pour it off.

• Dry the BRZ™ in a drying oven at 100 degrees C for one hour.

• Pulverize the sample.

• Send sample to Huffman Laboratories, Inc., 4630 Indiana St., Golden, CO 80403-1849 (303-278-4555).  Huffman will report the total nitrogen exchanged.

CATION EXCHANGE CAPACITY (CEC):

CEC (meqs/100gms) =	Nitrogen exchanged as % _____________________ 14.0067	x1000
	________________________________      .80

DISCUSSION

• The accepted test for CEC involves 5 immersions of the sample in AN-20.  Each immersion involves 1 day. Empirically one immersion corresponds to 80% of the actual CEC.  Five immersions have been avoided due to the time requirement.

• Drying the sample is very critical. The clinoptilolite contain free water and water of hydration. At 100 degrees centigrade different moisture contents are a function of time. Further, samples must be packaged immediately after removing an aliquot, because the clinoptilolite is a very effective desiccant.

• The samples are submitted to Huffman Laboratory of 4630 Indiana St., Golden CO., 80403 (phone 303-278-4455) for the total nitrogen exchanged. The procedure is described by Ed Hufffman Jr. as follows:

  • “Nitrogen is determined on a Thermo Flash EA 1112 analyzer. The technique is based on the classical Dumas method with thermal conductivity detection (TCD). The method is described in ASTM D5373 (coal)and ASTM D529 (petroleum products).

  • Weighed samples are combusted in oxygen at 950 degrees C. The combustion products (including N2 and NOx) are swept with a helium carrier gas through combustion catalysts, scrubbers and through a tube filled with reduced copper. The copper removes excess oxygen and reduces NOx to N2. The N2 is then separated from other gas on a chromatography column and measured with the TCD.

  • We use relatively large samples so the precision should be better than +- 0.1% absolute.”

MOISTURE DETERMINATION 

A composite sample is collected and the free moisture is determined in a drying oven set at 100-105 degrees C for two hours using an initial sample weight of 100 grams.

WEIGHTS

Weights are determined by calibrated scales for packaged product or by certified truck scales.

HEAVY METALS AND MINERALOGIC COMPOSITION 

Quoting the late George Desborough:

 “This work was done using the modem U. S. Geological Survey (USGS in Denver, CO) XRD equipment using the computerized JADE mineral identification programs to assist in identification of minerals. … More than 20 XRD samples (including composite samples from 3-15 foot thick zones at what is now the main mining pit of BRZ™) were studied. Quartz was never detected. Clinoptilolite was the only zeolite found. Opaline silica commonly referred to as “opal C-T” was the major diluent. Bulk chemical compositions were determined using XRF at USGS to determine concentrations of Na, Ca, K, Al, Si, Fe, Ti, P, etc. Energy dispersive analysis was used to quantitatively determine trace elements such as As, Se, Rb, Pb, Sr, etc.”