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Methods of Analysis

Cereals Canada uses approved methods of analysis developed by global organizations such as Cereals and Grains Association (AACC International Approved Methods of Analysis) when evaluating milling, wheat, flour and end-product quality. Additional methods developed and recognized within the industry are also used. Internal methods are developed with full transparency to ensure the delivery of reproducible and accurate results.

Cereals Canada – Methods of Analysis

All results are corrected to a 13.5% moisture basis (mb) for wheat and a 14.0% mb for flour or semolina unless otherwise specified.
AACC International Methods are from the Cereals and Grains Association: Approved Methods of Analysis, 11th Edition.

Alveograph values (corrected to 15.0% mb) are determined using the AlveoLab according to AACC International Method 54-30.02 using light mineral oil. Samples are evaluated one week after milling. The following curve parameters are measured: P (height x 1.1) is the resistance of the dough to deformation; L (length) is a measure of dough extensibility; P/L is the curve configuration ratio; W is the amount of work required to inflate the dough into a bubble; Ie (elasticity) measures the ability of the dough to return to its original shape; G (swelling) relates to the volume of air necessary to inflate the bubble until rupture.

Amylograph peak viscosity is determined using a Viscograph-E according to AACC International Method 22-10.01 with modifications.
Flour (65 g, 14% mb) and distilled water (450 mL) are placed in a bowl, mixed with a whisk and then added to the Viscograph-E.

Ash content is determined using AACC International Method 08-01.01. Samples are weighed into previously dried dishes
(600oC, minimum of 1 h). The samples are then incinerated overnight in a muffle furnace (600oC).

Internal Method

White pan bread is processed in a pilot scale bakery using a NTD baking procedure. Formulation, processing conditions, and equipment used are typical for commercial production of bread. All ingredients are mixed using a spiral mixer (2 min on slow speed, then on second speed until the dough is fully developed). The dough is then rested (10 min, ambient conditions), scaled into pieces (640 g) and rounded. The dough balls are rested (10 min), shaped using a commercial sheeter and moulder, panned and fully proofed (37°C, 85% RH). The samples are baked in a reel oven (200°C, 25 min).

Internal Method

White pan bread is processed in a pilot scale bakery using a sponge and dough baking procedure. Formulation, processing conditions,
and equipment used are typical for commercial production of bread. The sponge ingredients (a portion of flour, water, yeast, and yeast food) are prepared in a spiral mixer and then fermented in a proofing cabinet (27°C, 75% RH, 4 h). To prepare the dough, the fermented sponge and the remaining ingredients are placed in a spiral mixer and mixed on slow speed (2 min) and then on second speed until the dough is fully developed. The dough is rested (10 min, ambient conditions), scaled into pieces (640 g) and rounded. The dough balls are rested (10 min), shaped using a commercial sheeter and moulder, panned and fully proofed (37°C, 85% RH).
The samples are baked in a reel oven (200°C, 25 min).

Test baking using NTD method is based on AACC International Method 10-10.03 with modifications. All ingredients are placed in the bowl of a water-jacketed National MFG. Co. Swanson pin mixer (20oC, 118 rpm) which is controlled with software to measure mixing time (min) and energy (W) input. The dough is mixed 10% past peak time and placed in a covered bowl and allowed to rest (10 min, ambient conditions). The dough is scaled (165 g), rounded by hand and allowed a second rest (10 min, ambient conditions). The dough is sheeted, moulded, panned and proofed (37oC, 85% RH) to a fixed height. Samples are baked in a reel oven (204oC, 20 min).

Test baking using a LTF method is based on AACC International Method 10-10.03 with modifications. All ingredients are placed in the bowl of a water-jacketed National MFG. Co. Swanson pin mixer (15°C, 118 rpm) which is controlled with software to measure mixing time (min) and energy (W) input. The dough is mixed 10% past peak time and scaled (165 g), rounded, and allowed to rest in a fermentation cabinet (37°C, 85% RH; 105 min). After the initial fermentation, the first punch is performed by sheeting, tri-folding and placing the dough back into the fermentation cabinet for a second rest period (37°C, 85% RH; 50 min). The second punch is handled the same way as the first punch and the dough is placed back into the fermentation cabinet (37°C, 85% RH; 25 min). After 180 minutes of total fermentation time, the dough is sheeted, moulded, panned and proofed (37°C, 85% RH) to a fixed height. Samples are baked in a reel oven (204°C, 20 min).

Assessment of the crumb colour of a bread slice is performed using the Minolta colorimeter (D65 illuminant, 2o standard observer angle) according to manufacturer’s instructions. Two slices of bread are placed on the light projection tube and the measurement
is taken. L* values (0 = black to 100 = white), which indicate the brightness of the crumb, are recorded.

Assessment of flour/semolina colour is performed on a slurry of flour/semolina and water using the glass ended attachment according to AACC International Method 14-30.01 with respect to flour weight, volume of water, mixing time and waiting time. Colour is measured one week after milling. The Minolta colorimeter (D65 illuminant, 2o standard observer angle) is used according to manufacturer’s instructions and the following parameters are measured: L* (0 = black to 100 = white); a* (-a* = green to +a* = redness); b*
(-b* = blue to +b* = yellow).

Colour of a noodle sheet (see Noodle Processing for details) is measured using a Minolta colorimeter (D65 illuminant, 2°
standard observer angle). The dough sheet is folded into six layers and stored in a covered container at ambient
conditions. The following parameters are measured: L* (0 = black to 100 = white); a* (-a* = green to +a* =
red); b* (-b* = blue to +b* = yellow). The average of five colour measurements, taken at five spots on the dough
sheet surface at 3 and 24 h from mixing time, are reported.

Assessment of semolina colour is performed using a granular material attachment and the Minolta colorimeter (D65 illuminant,
2o standard observer angle) according to manufacturer’s instructions. Samples are evaluated one week after milling. The following parameters are measured: L* (0 = black to 100 = white); a* (-a* = green to +a* = red); b* (-b* = blue to +b* = yellow).

A Minolta colorimeter (D65 illuminant, 2o standard observer angle) is used to measure the colour of dried spaghetti strands (see Spaghetti Processing for details). Strands are mounted on standard white cardboard (7.5 cm x 7.5 cm) using double sided tape. The following parameters are measured: L* (0 = black to 100 = white); a* (-a* = green to +a* = red); b* (-b* = blue to +b* = yellow).

Dried spaghetti (30 g, 1 cm length) is cooked in boiling water (300 mL) to its optimal cooking time (OCT) which is defined as the time when the center core of the spaghetti just disappears when pressed between two Plexiglas plates. After the OCT is reached, the spaghetti is drained and rinsed with 100 mL water. The cooking container is rinsed with an additional 100ml water, and the cooking
and rinse water is retained. The cooking water is evaporated (130oC, 24 h) and the remaining residue is weighed and expressed
as a percentage of the initial spaghetti weight.

Crumb structure is evaluated using C-Cell imaging according to AACC International Method 10-18.01. An average of the measurements taken on two slices of bread from the centre of the loaf are reported.

Extensographs are performed using the Extensograph-E according to AACC International Method 54-10.01 with the modification that
the dough test pieces are not stretched at 90 min, only re-formed. Results are reported for the stretches completed at 45 and 135 min.
The Extensograph-E is calibrated so that a 100 g load is equivalent to 80 BU. Samples are tested one week after milling. The following parameters are measured: Rmax is the maximum height (maximum resistance) of the curve; E is a measure of the extensibility;
A is the area under the curve (energy).

Falling Number is determined using the FN1000 with the Shakematic 1095 according to AACC International Method 56-81.03.
For evaluation of wheat FN, a sample of wheat (minimum of 250 g) is ground using the FN3100 laboratory mill with 0.8 mm screen.

Farinographs are performed using the Farinograph-TS or Farinograph-AT with either the large bowl (300 g) or small bowl (50 g) according to AACC International Method 54-21.02. Flour is tested one week after milling. The following parameters are measured: water absorption (FAB) is the amount of water needed to center the curve on the 500 BU line at maximum consistency (peak); dough development time (DDT) is the time for the dough to reach maximum consistency (peak); stability is the amount of time that the top portion of the curve is above the 500 BU line; mixing tolerance index (MTI) is the drop in BU of the top of the curve at DDT to the top of the curve 5 min after DDT.

Dried spaghetti (12 strands, 5 cm length) is cooked in boiling water (250 mL, 9 min). After cooking, the spaghetti is drained and placed on a fine sieve. A TA.XT plus texture analyzer with a blade (TA-47) is used to measure firmness (45 s and 115 s after cooking). The average of four measurements is reported for each sample.

Wheat for milling is cleaned using a dockage tester with standard screens and then conditioned for 20 to 24 hours, based on wheat class: hard wheats (i.e. CWRS; 16.5% moisture); medium hard wheats (i.e. CPSR, CWRW; 16.0% moisture). Milling is done using a Bühler laboratory flour mill using preset feed rates and roll gap settings for all common wheat classes. After milling, the bran and shorts fractions are put through a Bühler bran finisher and any additional flour released is added to the original flour and used for calculation of the final flour yield based on total products.

Correction of flour milling yield to a 0.50% ash basis is calculated to show milling yields on a constant ash
basis and allows for a better comparison among wheat samples with different extraction rates and flour
ash contents. The correction is based on an estimate derived from a laboratory mill ash curve where each
0.01% difference in flour ash content (based on a 0.50% ash content) is equal to a 0.50% extraction
adjustment. It is calculated as follows:

Semolina granulation is determined using a Ro-tap sieve shaker according to AACC International Method 66-20.01 with modifications.

The BVM 6600 bread volume meter is used to measure loaf volume according to AACC International Method 10-14.01.
Loaf weight is also determined. Specific volume is calculated as the ratio of loaf volume to loaf weight.

Noodles (16 strands, 10 cm length) are assessed for texture by cooking in boiling water (500 mL) at three different cooking times (2.5, 3.5, 5.0 min). After each cooking time, the noodles are drained, cooled in water (22oC, 1.5 min) and placed on a sieve. The cooled noodles are lined up on the sieve and transferred to the TA.XT plus measuring plate within an allotted amount of time (3.75 min) prior to taking a measurement. A TA.XT plus texture analyzer with a blade (TA-47) is used to measure firmness, maximum cutting stress and elasticity index. An average of two measurements is reported for each sample at each cooking time.

Mixolab assessment is determined using the Mixolab 2 according to AACC International Method 54-60.01. Flour is tested one week after milling. The following parameters are measured: water absorption (WA) is the amount of water needed to form dough with a consistency of 1.1 ± 0.05 Nm at the C1 torque; C1 torque (C1) is initial peak dough consistency; time to T1 (T1) is the time needed to reach C1; Stability is the time around C1 where the torque is greater than C1-11%; CS time; is the time required for the consistency to drop by 50% after heating has started; C2 torque (C2) represents the lowest point of the curve; C3 torque (C3) is the maximum torque obtained after C2 during the heating phase; C4 torque (C4) is the minimum torque obtained after C3; C5 torque (C5) is the torque at the end of the test.

The moisture content of a sample of bread is determined according to AACC International Method 62-05.01 and AACC International
Method 44-11.01.

The moisture content of ground wheat/flour/semolina is determined according to AACC International Method 44-15.02 using the single stage procedure (130oC, 1 h).

The moisture content of whole kernel wheat is determined using the AM5200-A according to AACC International Method 44-11.01.

Ingredients are mixed (100 rpm, 10 min) using a pilot scale Ohtake vertical vacuum mixer. The noodle sheets are prepared using a pilot Ohtake noodle line starting with a gap setting of 5.1 mm. The dough sheet is then subjected to four reduction passes (2.0, 1.5, 1.2, 1.0 mm) and cut into noodle strands at the final pass. The cut noodle strands are continually fed into a traveling net conveyor and cooked with steam while passing through a tunnel steamer. Noodles are cut into a predetermined length to make one serving size. Noodle portions are deep-fried in a tunnel fryer and then cooled to room temperature in a cooling tunnel.

YAN are processed using a laboratory scale Ohtake vertical mixer and laboratory scale Ohtake sheeter. A flour and salt solution are mixed (100 rpm, 10 min) and rested (15 min). Sheeting begins with a gap setting of 3.5 mm and then the dough sheet is folded, sheeted again at the same gap setting and rested (30 min) on the noodle roller in a plastic bag. The dough sheet is subjected to four reduction passes (2.0, 1.4, 1.1, 0.9 mm) and a final gap setting is adjusted to ensure the resulting dough sheet has a thickness of 1.4 mm. A section (180 cm) is cut from the dough sheet for colour (see Colour – Noodle for details). The remaining dough sheet is cut into noodle strands using a No. 10 cutter to produce noodles with a width of 3.0 mm.

WSN are processed using an Ohtake vertical mixer and laboratory scale Ohtake sheeter. A flour and salt solution are mixed (100 rpm, 10 min) and rested (15 min). Sheeting begins with a gap setting of 3.5 mm and the dough sheet is folded, sheeted again at the same gap setting and rested (30 min) on the noodle roller in a plastic bag. The dough sheet is subjected to four reduction passes (2.0, 1.5, 1.2, 1.0 mm) and a final gap setting is adjusted to ensure the resulting dough sheet has a thickness of 1.4 mm. A section (180 cm) is cut from the noodle sheet for colour (see Colour – Noodle for details). The remaining dough sheet is cut into noodle strands using a No. 10 cutter to produce noodles with a width of 3.0 mm.  To produce dried WSN noodles, cut noodles are placed on rods and hung to dry in an Ohtake pilot dryer for 7 h.

Wheat kernel hardness is assessed by determining the PSI using AACC International Method 55-30.01 with modifications. Wheat, with moisture content between 11.0-13.0%, is ground using an UDY Cyclone grinder (1.0 mm screen) and a feed rate regulator (52 rpm). Ground wheat is sieved using a Ro-tap sieve shaker.

Protein content (N x 5.7) is measured using a combustion nitrogen analysis (CNA) method with the LECO FP-828 according to Williams et al. (Protein testing methods. In, Wheat Protein, Production and Marketing. Proceedings of the Wheat Protein Symposium. Saskatoon, SK. University of Saskatchewan Press. March 9-10, 1998. pp. 37-47). Drift corrections are done using EDTA.

Wheat for milling is cleaned using a dockage tester with standard screens and then conditioned for 16 to 20 hours. Milling is done using a Bühler laboratory semolina mill using preset feed rates and roll gap settings. After milling, the semolina is purified using Namad laboratory purifier. Break flour is added to purified semolina and the total amount is reported as semolina yield. To calculate total yield, sizing flour is added to purified semolina and break flour blend. Yields are calculated based on total products.

A shock test is performed to determine how bread dough can tolerate the mechanical stress or abuse present in a commercial production line. A fully proofed bread dough is dropped in its pan from a specified height (3.5 – 4.0 cm) onto a solid, flat surface and evaluated for signs of collapsing. Specific volume is measured using the BVM 6600 bread volume meter (see Loaf and Specific Volume – Bread for details). Results are recorded as the specific volume of the shocked loaf compared to the specific volume of the non-shocked loaf to determine dough recovery in the oven.

A Namad laboratory pasta extruder with a Teflon die (1.80 mm diameter) is used to process spaghetti. Semolina and water (31% absorption based on semolina weight) are mixed with a paddle mixer (12 min) then the dough is extruded under vacuum. Spaghetti is dried in a Bühler batch dryer using a high temperature drying cycle (85oC, 5.5 h).

Speck count in semolina is determined using rar-SpeckCnt software. A sample of semolina is placed in a square sample holder (17.5 cm x 17.5 cm) that has a glass top and compressed to approximately 1 cm thickness. The sample holder is scanned using a flatbed scanner to provide a 10 x 10 cm image which is processed by the software for speck counting. The specks identified are categorized by their darkness (low, medium, high) and size (small, medium, large).  Total specks, dark specks and large specks are recorded for each test which is done in 4 replicates. The average of the results is determined, divided by two and expressed as the number of specks per 50 cm² of semolina.

Starch damage is measured using the SDmatic according to AACC International Method 76-33.01.

Evaluation of the starch pasting profile of flour is performed using the RVA 4500 according to AACC International Method 76-21.02 (STD1, 13 min profile). The following parameters are measured: peak viscosity is the maximum viscosity during the heating cycle; peak time is the time at peak viscosity; pasting temperature is the temperature where a rapid increase in viscosity occurs; hot paste viscosity is the minimum viscosity observed during the heating period; breakdown is the difference between peak and hot paste viscosities; final viscosity is the viscosity at the end of the test; setback is the difference between final and hot paste viscosities.

Ingredients are mixed using a GRL-1000 mixer (45 rpm, 0.5 min) and then at a higher speed (105 rpm) until dough is developed. The dough is rested (15 min) and sheeted (20 passes, 5.5 mm gap). The dough sheet is subsequently rolled into a cylinder and six dough pieces are scaled (150 g each) and rounded by hand. The dough pieces are placed in a covered steaming tray, proofed (45 min, 32oC, 85% RH), and steamed (25 min, 100°C) in a commercial steamer.

Steamed breads are weighed and measured for height and width. Volumes are determined by rapeseed displacement. The colour of the steamed bread skin is measured by a Minolta colorimeter (D65 illuminant). The following parameters are measured: L* (0 = black to 100 = white); a* (-a* = green to +a* = red); b* (-b* = blue to +b* = yellow). Breads are subjectively scored using an internal method. Steamed breads are evaluated for physical attributes of exterior appearance, crumb structure and colour, texture and overall acceptability.

Pan bread is subjectively scored using an internal method to obtain the total bread score. Total bread score is the sum of the score for external loaf characteristics (symmetry, crust character, crust colour, and break and shred) and the score for internal crumb characteristics (crumb colour and crumb structure).

Flour (300 g) is mixed with 36% water (w/w) in the GRL 1000 Mixer (6 min, 105 rpm) to produce a homogeneous dough crumb. Dough crumbs are sheeted using a laboratory scale Ohtake sheeter with a gap setting of 3.5 mm, followed by a lamination step at the same gap setting. The dough sheet is rested (10 min) in a plastic bag and then subjected to four reduction passes (2.0, 1.5, 1.2, 1.0 mm). The resulting noodle sheet is sealed in a plastic bag to prevent moisture loss. Colour measurements are taken on the folded dough sheet (6 layers) at 2 and 24 h using a Minolta colorimeter (D65 illuminant 2o standard observer angle). The following parameters are measured: L* (0 = black to 100 = white); a* (-a* = green to +a* = red); b* (-b* = blue to +b* = yellow).

Wet gluten content and gluten index values are determined using the Glutomatic 2000 with the Gluten Index Centrifuge 2015 according to AACC International Method 38-12.02. The single-stage washing procedure is used for flour while the two-stage washing procedure is used for semolina/ground wheat. Flour/semolina samples are tested one week after milling.

Semolina yellow pigment content is determined according to Fu et al. (2013. J. Cereal Sci. 57: 560-566; doi: 10.1016/j.jcs.2013.03.007).

For more information contact:

Norbert Cabral
Manager, Milling
204-983-2171 / ncabral@cerealscanada.ca

Kristina Pizzi
Manager, Analytical Services
204-984-6076 / kpizzi@cerealscanada.ca

Lindsay Bourré
Manager, End-products
204-984-1063 / lbourre@cerealscanada.ca

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