Flaked or expanded cereals

26
Cereals
CONTENTS
METHODS OF ANALYSIS (BOE 19/07/1977 and 07/20/1977) 1. 2. 3. 4. 5. 6. 7. 8. 9. 1
0. 11. 12. 13. 14. 15. 16. 17. 18. 19. Determination of the cellulosic material
........................................... Humidity ...........................
.................. Ash ................................................ Protein
............................................... Fat ............................
..................... .. Maltose Index ................................. Fat aci
dity ........................................ Oxidizing agents (reaction with po
tassium iodide) ..................................... Bromate and iodate in flou
r (Qualitative method) ............................... Benzoyl Peroxide (Qualita
tive method with benzidine) ...................................... Pelshenke Ind
ex .............................. Gluten .......................................
.......... . Brabender Farinograph .......................... Alveograph Chopin
(Provisional) ............. Determining the extent of deposition (as Zeleny) ...
............ Ascorbic Acid (Vitamin C) (Qualitative method) (BOE 08/29/1979) Amm
onium persulfate (Qualitative Method) (BOE 07/20/1977) .................. ......
....... Phosphorus (B.O.E. 08/29/1979) ................... Detection and quantif
ication of common wheat flour (Triticum vulgare) in semolina and pasta .........
...... Detection of flour degraded by the attack of Pentatomidae ...............
....
7 9 9 10 11 12 13 14 14 15 15 15 16 17 20 21 21 21
23 25
20.
Flaked or expanded cereals
METHODS OF ANALYSIS (B.O.E. 20/01/1988) 1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. S
ample Preparation ................... Humidity .................................
............ Ash ................................................ Fat ..........
....................................... .. Proteins ............................
.................. Insoluble fiber ..................... Crude fiber ...........
................................ Sugar .........................................
..... Chloride ............................................... Zinc ............
..................................... ..... Lead ...............................
.................. .. Mercury ............................................... 27
27 27 28 29 30 31 32 34 35 36 36
13. Copper ................................................. . 14. Arsenic .....
..........................................
37 38
Beer
METHODS OF ANALYSIS (B.O.E. 10/23/1985) 1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 1
3. 14. Alcohol .......................... Real extract .........................
................ Dry extract primitive ......................... Degree of ferme
ntation ......................... Total acidity ................................
.......... Carbon dioxide (CO2) ..................... pH .......................
.......................... ....... Ash .........................................
....... Phosphoric acid ...................................... Sulfur Dioxide ..
............................. Copper ...........................................
...... .. Zinc ................................................. .... Carbohydra
tes ............................. Color ........................................
......... ... 45 51 68 69 69 70 71 72 72 74 75 76 76 77
Pasta
METHODS OF ANALYSIS (B.O.E. 08/09/1987) 1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 1
3. 14. Sample preparation. see page Humidity ........................... Ash ...
........................... see page Fat ............................... see pag
e Proteins ............................ see page see page insoluble fiber food .
. Crude fiber ......................... see page see page Sugars ...............
............. see page Chloride ............................. see page acidity l
evel ................................... Lead ................................ s
ee page Mercury ............................ see page Copper ...................
............. Arsenic ............................. see page see page 27 * 27 *
27 * 28 * 29 * 30 * 31 * 32 * 34 * 41 * 36 * 36 * 37 * 38 *
* Coincide exactly with the tests or Expanded Cereal Flakes, described on the pa
ge indicated.
Cookies
METHODS OF ANALYSIS (B.O.E. 24/11/1987) 1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 1
3. 14. Sample preparation .. see page Humidity ........................... Ash .
............................. see page Fat ............................... see p
age Proteins ............................ see page see page insoluble fiber food
.. Crude fiber ........................ see page see page Sugars ..............
.............. see page Chloride .............................€see page fat extr
action for identification ................................... Lead .............
................... see page Mercury ............................ see page Coppe
r ................................ Arsenic ............................ see page
see page 27 * 27 * 27 * 28 * 29 * 30 * 31 * 32 * 34 * 43 * 36 * 36 * 37 * 38 *
List of reagents and ancillary products used in analytical methods, Cereals, Gra
ins and Beer .... 78 additives and processing aids for use by industrial food ..
...................................
82
* Coincide exactly with the tests or Expanded Cereal Flakes, described on the pa
ge indicated.
M
METHODS OF ANALYSIS (B.O.E. 20/01/1988) 1. SAMPLE PREPARATION 1.1. Principle. Ho
mogenization and reduction of sample size for the proper conduct of the analysis
. 1.2. Material and apparatus. 1.2.1. Grinding apparatus that does not cause war
ming, easy to clean, and to provide particle size between 800 and 1,200 μ. 1.2.2
. Containers of adequate capacity with hermetic seal to preserve the sample. 1.3
. Procedure. 1.3.1. Sample in a single package: to homogenize the sample. Take a
minimum of 200 g crush in the apparatus described in 1.2.1. and re-mix. 1.3.2.
Sample in several envases.Homogeneizar the portion contained in each package, ta
ke equal amounts of each to finally obtain a minimum of 200 g of sample. Blend i
n the apparatus described in 1.2.1. and re-mix. 1.4. Remarks. Sample preparation
, this will serve as the basis for all determinations, except where specifically
mentioned against, trying to make the preparation of the analysis in the shorte
st possible time. The effectiveness of ventilation is determined with the help o
f grits as test material, which has a maximum particle millimeter. The ventilati
on shall be such that, simultaneously drying at 130 ° C all samples that the ran
ge can contain, first for two hours and then for three hours, the results show a
difference between them less than 0.15 per 100 in absolute value. 2.2.4. Desicc
ator effective drying agent. 2.3. Procedure. Weigh to the nearest 1 mg, about 5
g of sample in a weighing bottle, previously prepared by method 1. Enter the wei
ghing bottle on the stove (2.2.3.) At 130 ° C ± 1 ° C and uncover. Keep in the o
ven for one hour and thirty minutes. Cover the weighing bottle before removing f
rom the oven and let cool at room temperature in desiccator and weigh below. 2.4
. Calculations. The moisture of the sample expressed in percent is given by the
following formula: (P1 - P2) 100 H% = ------- P Where: P1 = weight in grams, of
the weighing bottle with the sample. P2 = weight in grams, of the dried sample w
eighing bottle. P = weight in grams, of the sample. The resulting difference bet
ween duplicate determinations of the same sample should not exceed 0.1% in absol
ute value. 2.5. References. 2.5.1. Methods of the International Association for
Cereal Chemistry (ICC). 2.5.2. AOAC, M. 14 003 1980.
2. MOISTURE 2.1. Principle. Determine the weight loss of sample when subjected t
o heating in an oven under specific conditions. 2.2. Material and apparatus. 2.2
.1. Analytical balance accurate to 0.1 mg. 2.2.2. Metal or glass weighing bottle
with a lid and a surface allowing distribution of the sample of more than 0.3 g
/cm2. 2.2.3. Heated temperature electric heating, possibly forced air, regulated
so that the air temperature inside is 130 ° C and has enough ventilation. The s
tove will heat capacity such that previously regulated the temperature of 130 °
C, can reach that temperature again in half an hour after placing both inside th
e maximum number of samples to dry.
3. ASH 3.1. Principle. 3.1.1. Definition. Residue obtained by incineration at a
temperature of 550 ± 10 ° C until complete combustion of organic matter and obta
in a constant weight. 3.2. Material and apparatus. 3.2.1. Crucibles not targeted
in the test conditions, with a minimum size of 40 mm in height and 45 mm higher
.
27
3.2.2. Hotplate. 3.2.3. Electric (muffle) with temperature control device. 3.2.4
. Desiccator capable of containing an efficient drying agent, such as 141 219 Ca
lcium chloride anhydrous, escoriforme PRS 141 154 PRS pentaoxide di-Phosphorus a
nd Silica Gel 211 335 3-6 mm with indicator QP. 3.3. Procedure. Weigh 1 mg of 2-
6 g of sample prepared using the official method number 1, previously incinerate
d in a crucible and weighed.€Place the crucible and its contents on a hot plate,
taking care that the combustion is not too fast, so no loss of solid matter by
projection. Take then the crucible to the muffle (550 ± 10 ° C) until complete c
ombustion of the substance (white or gray ash.) Cool to room temperature in a de
siccator. Weigh below. 3.4. Calculations. 3.4.1. The ash content of natural subs
tance is given by the following formula: P1 - P2% ash = ---- x 100 P Where: P1 =
weight in grams of the crucible with the ash. P2 = weight in grams of the empty
crucible. P = weight in grams of the sample. 3.4.2. The ash content of dry matt
er is given by the following formula: C x 100% ash = ---- 100 - H where: C =% as
h obtained in (3.4.1.). H = Humidity. In both cases the results will be consider
ing only the first decimal place. 3.5. Remarks. 3.5.1. If necessary, to obtain a
uniform burning the sample may be moistened before ethanol preincineración 95 1
00 or ash-free vegetable oil. 3.5.2. If the test sample contains chloride added,
deduct the value of ash obtained by the former's share of them.
3.5.3. Limit mistakes. When the ash content does not exceed 1 per 100 in the sam
ple, the difference in the results of a test performed in duplicate must not exc
eed 0.02 per 100. If the ash content exceeds 1 per 100, the difference should no
t exceed 2 per 100 of such content. If more than repeat the determination. 3.6.
References. 3.6.1. AOAC, 1980 edition, 14 006.
4. FAT 4.1. Principle. The product is hydrolyzed with dilute hydrochloric acid.
Dry mass resulting fats are extracted with ether, the solvent evaporated and the
residue weighed. 4.2. Reagents. 131 019 Hydrochloric Acid 35% PA-ISO 131 074 13
2 770 Water PA-ACS diethyl ether stabilized with ~ 6 ppm of BHT PA-ACS-ISO 211 8
35 131 459 Pumice granules QP Silver Nitrate PA-ACS-ISO 4.2.1. Hydrochloric acid
3N. Dilute Hydrochloric Acid 35% PA-ISO in PA-ACS water until the concentration
indicated. 4.2.2. Diethyl Ether stabilized with ~ 6 ppm of BHT PA-ACS-ISO, free
 from peroxides. 4.2.3. Silver Nitrate Solution. Dissolve a few grams of Silver
Nitrate PA-ACS-ISO 1000 ml of water in PA-ACS. 4.3. Material and apparatus. 4.3.
1. Soxhlet type extractor. 4.3.2. Drying oven capable of maintaining constant te
mperature of 100 ° C ± 1 ° C. 4.3.3. Desiccator effective drying agent. 4.4. Pro
cedure. Weigh 1 mg, about 10 g of sample prepared using the official method (par
agraph 1) in a flask of 250-300 ml. Stirring continuously, add 100 ml of 3N hydr
ochloric acid (4.2.1.), Add a few glass beads or granules Pumice QP washed and d
ried and closed with glass stopper tightly-fitting glass or clock. Boil about si
xty minutes, stirring occasionally, cool and filter through moistened filter. Wa
sh the precipitate with PA-ACS water until the filtrate gives no precipitate wit
h silver nitrate or acid reaction of litmus paper. Put the filter in a dish and
dry in oven at 100 ° C ± 1 ° C.
28
M
Dry the filter and placed in a Soxhlet type extractor cartridge is plugged with
cotton and degreasing. The cartridge is placed in the extractor and pour the eth
er stabilized with ~ 6 ppm of BHT PA-ACS-ISO, leaving siphon about eight hours.
The receiving flask should be dried and weighed. Evaporate the solvent, dried in
an oven and weigh. 4.5. Calculations. 4.5.1. The fat content in natural substan
ce is given by the following formula: P1 - P 2% fat = ---- x 100 P Where: P1 = w
eight in grams of fat flask. P2 = weight in grams of the flask. P = weight in gr
ams of the sample. 4.5.2. The fat content of dry matter is given by the followin
g formula: G x ---- 100% fat = 100 - H where: G = percentage of fat obtained in
4.5.1. H = Humidity. 4.6. Remarks. 4.6.1. To perform the above procedure may be
used or semi-automatic systems, adapting to the equipment specifications. 4.7. R
eferences. 4.7.1. AOAC, 1980 edition, 14 059. 251170 121085 171327 131532 171617
141625 131687 131716 Methylene Blue (CI 52015) DC Ethanol 96% v / v PA RE Pheno
lphthalein solution 1% Potassium Sulphate PA-ACS-ISO Methyl Red (CI 13 020) RE-A
CS Sodium Selenium metal powder PRS hydroxide lentils PA-ACS-ISO Sodium sulfate
anhydrous PA-ACS-ISO
5.2.1. Sulfuric Acid 96% PA-ISO free of nitrogen. 5.2.2. 40% sodium hydroxide. D
ilute sodium hydroxide lentils PA-ACS-ISO with PA-ACS water until the concentrat
ion indicated. 5.2.3. Catalyst.€(Mix 5 g of anhydrous sodium sulphate PA-ACS-ISO
or Potassium Sulphate PA-ACS-ISO with 5 mg of selenium metal powder PRS). You c
an also use another suitable catalyst. 5.2.4. Phenolphthalein indicator solution
1% RE. 5.2.5. Taschiro indicator. Mix 20 mg of Methyl Red (CI 13 020) RE-ACS an
d 10 mg Methylene Blue (CI 52015) DC in 100 ml of ethanol 96% v / v PA. You can
also use Methyl Red (CI 13 020) RE-ACS prepared in the proportion of 0.5% in Eth
anol 96% v / v PA. 5.2.6. 4% boric acid solution IR. 5.2.7. Sulfuric acid 0.05 m
ol / l (0,1 N) SV or hydrochloric acid 0.1 mol / l (0,1 N) SV. 5.3. Material and
apparatus. 5.3.1. For digestion. 5.3.1.1. Kjeldahl flasks or similar type. 5.3.
1.2. Battery electric blankets or similar. 5.3.2. For distillation. 5.3.2.1. Ste
am generator flask. 5.3.2.2. Refrigerant. 5.3.2.3. Receiving flask. 5.3.3. Degre
e. 5.3.3.1. Burette automatic burette glass. 5.4. Procedure. Weigh to the neares
t 1 mg, about 0.5 to 2.5 g of sample, prepared using the official method number
one, put it in the Kjeldahl flask (5.3.1.1.). Add about 5 g of the catalyst (5.2
.3.) Sulfuric acid 20 ml of 96% PA-ISO (the amount varies in protein and fat con
tent of the sample). Putting digest in 5.3.1.2., Being careful not to raise the
top temperature too until the cessation of the shedding of the foam (if necessar
y add a small amount of paraffin). Digested until the solution is clear. Cool, d
ilute, add a few drops of Phenolphthalein solution 1% RE and connect the distill
ation apparatus by adding 40% sodium hydroxide (5.2.2.) To turn. In the receivin
g flask to 100 ml of 4% boric acid solution with a few drops of RE indicator (5.
2.5.), Taking care that the end of the refrigerant fluid is well covered.
5. PROTEIN 5.1. Principle. Determination of nitrogen, converting the organic nit
rogen present in ammonium sulfate with sulfuric acid. After alkaline with sodium
 hydroxide, distilled collecting the distillate in boric acid, ammonia titration
collected N/10 acid. 5.2. Boric Acid Reagents 172 222 RE 181 023 4% solution hy
drochloric acid 0.1 mol / l (0,1 N) SV 131 058 96% Sulfuric Acid 181 061 PA-ISO
Sulphuric Acid 0,05 mol / l (0,1 N) SV Water PA-131 074 ACS
29
Keep the distillation about 15 minutes (or more if necessary, until basic reacti
on) and flushing the coolant and head end of the distillate with Sulphuric Acid
0,05 mol / l (0,1 N) SV 0 Hydrochloric Acid , 1 mol / l (0,1 N) SV. Make a targe
t. 5.5. Calculations. 5.5.1. The protein content of natural material is given by
the following formula: 0.14 x 6.25 (V1 - V0)% protein = ---------- P Where: V1
= Volume, in ml of hydrochloric acid or sulfuric acid 0.1 N 0.1 N used in the de
termination. V0 = Volume, in ml of 0.1 N hydrochloric acid or sulfuric acid 0.1
N used in white. P = weight in grams of the sample. 5.5.2. The protein content i
n dry matter is given by the following formula: px ---- 100% protein = 100 - H w
here: p =% proteins obtained in 5.5.1. H = Humidity. 5.6. Remarks. 5.6.1. The di
fference between two successive determinations expressed as% protein should not
exceed 0.25%. 5.6.2. To make the procedure may be used Kjeldahl or semi-automati
c systems, adapting to the equipment specifications. 5.7. References. 5.7.1. AOA
C (1980) 2057. 5.7.2. Pearson, 5th edition (1962).
6.2. Material. 6.2.1. Thermostatic bath and reflux condenser. 6.2.2. Filtering g
lass filters 2. 6.2.3. Filtration systems by vacuum suction. 6.2.4. Desiccator.
6.2.5. Oven for 37 ° C and 110 ° C. 6.2.6. Electric (muffle) with temperature co
ntrol device. 6.2.7. Precision balance. 6.3. Reagents. Acetone 131 007 PA 131 66
9-ACS-ISO Ethylenediaminetetraacetic acid disodium salt 2-hydrate PA-ACS-ISO 131
032 ortho-Phosphoric Acid 85% PA-ACS-ISO 131 074 Water PA-ACS-amylase type VI-A
161 805 decahydronaphthalene, mixture of isomers PS 141 317 ethyl ether Ethylen
e glycol mono-di-PRS 131 644 Sodium tetra-Borate 10-hydrate PA-ACS-ISO 122 363 P
A Sodium Sulfate Sodium dodecyl di-hydrogen phosphate anhydrous 131 679 di-Sodiu
m hydrogen phosphate anhydrous 131 717 PA-ACS Anhydrous Sodium Sulfite-PA ACS 6.
3.1. Sodium dodecyl sulphate PA. 6.3.2. Ethylenediaminetetraacetic acid disodium
salt 2-hydrate PA-ACS-ISO. 6.3.3. di-Sodium tetra-Borate 10-hydrate PA-ACSIS. 6
.3.4. Ethyl ether Ethylene glycol mono-PRS. 6.3.5. Decahydronaphthalene, mixture
of isomers PS. 6.3.6. Sodium Sulfite anhydrous PA-ACS. 6.3.7. di-Sodium Hydroge
n Phosphate anhydrous PAACS. 6.3.8. di-Sodium tetra-Borate 10-hydrate PA-ACSIS 6
.3.9. Acetone PA-ACS-ISO. 6.3.10. -Amylase type VI-A (Sigma A-6880 or equivalent
). 06/03/1911. Ortho-Phosphoric Acid 85% PA-ACS-ISO.€06/03/1912. Detergent solut
ion: mix 18.61 g ethylenediaminetetraacetic acid disodium salt 2-hydrate PA-ACS-
ISO and 6.81 grams of di-Sodium tetra-Borate 10-hydrate PA-ACS-ISO with 150 ml o
f water-PA ACS and heat until dissolved. Dissolve 30 g of sodium dodecyl sulfate
and 10 ml PA mono-ethyl ether of ethylene glycol in 700 ml PRS PA-ACS hot water
and mix with the previous solution. Dissolve 4.56 g of di-Sodium Hydrogen Phosp
hate anhydrous PA-ACS in 150 ml of water and mix PA-ACS with previous solutions.
Adjust to pH 6.9 to 7 with ortho-Phosphoric Acid 85% PA-ACS-ISO, if necessary.
6. Insoluble Fibre 6.1. Principle. The sample is extracted with a detergent solu
tion hot. The residue was incubated with amylase solution and filtered. The dete
rmination of ash in the waste filtering allows us to know, by weight difference,
the amount of cellulose, hemicellulose and lignin in the sample.
30
M
06/03/1913. 0.1 N buffer: Mix 39.2 ml of sodium di-hydrogen phosphate anhydrous
0.1 M (prepared by dissolving 13.6 g in 1 liter of water PAACS) with 60.8 ml of
Sodium Phosphate 0.1 M di-Base (prepared by dissolving 14.2 g in 1 liter of wate
r PAACS). 6.4. Procedure. Weigh 1 mg, about 1 g of sample prepared by method 1.
Orderly Add 100 ml of detergent solution, 2 ml of decahydronaphthalene, mixture
of isomers PS and 0.5 g anhydrous sodium sulphite PAACS (6.3.6.). Heat to boilin
g and maintained under reflux for one hour. Filter through sintered glass filter
# 2 (previously calcined at 550 ° C) connected to a vacuum suction system. Wash
ed successively with 300 ml of PA-ACS boiling water. Add to exceed the level of
residue, a 2.5% solution of amylase in phosphate buffer 0.1 N Incubate at 37 ° C
for 18 hours or so. Filter the enzyme solution by suction through a vacuum and
wash the residue with 80 ml of acetone PA-ACS-ISO. Dry the filter and residue at
110 ° C for 8 hours at least. Cool in desiccator. Keep the filter with the resi
due in flask at 550 ° C for three hours. Cool and weigh. 6.5. Calculations. The
insoluble dietary fiber content in% is given by the following formula: P1 - P2 x
100% = insoluble fiber P0 ------- Where: P0 = weight in mg of the sample. P1 =
weight in mg of dried residue + crucible at 110 ° C. P2 = mg Weight of crucible
+ residue burned. 6.6. Remarks. 6.6.1. Samples containing more than 10% fat shou
ld be degreased before. 6.6.2. To use the above procedure may be used or semi-au
tomatic systems adapted to the specifications of the equipment. 6.7. References.
6.7.1. AACC Method, 1932-1920 (1979). 7. Crude fiber 7.1. Principle. Treating t
he sample, degreased if necessary, with sulfuric acid solutions and potassium hy
droxide of known concentrations. Separate the residue by filtration, washing, dr
ying and weighing the insoluble residue, subsequent measurement of mass loss on
ignition at 550 ° C. 7.2. Material and apparatus. 7.2.1. Glassware commonly used
in laboratory. 7.2.2. Crucible 2. 7.2.3. Muffle furnace thermostat. 7.2.4. Desi
ccator effective drying agent. 7.2.5. Oven, capable of maintaining constant temp
erature of 130 ± 1 ° C. 7.2.6. Filtering equipment. 7.3. Reagents. Acetone 131 0
07 PA-ACS-ISO 131 058 96% Sulphuric Acid PA-ISO 131 074 132 770 Water PA-ACS die
thyl ether stabilized with ~ 6 ppm of BHT PA-ACS-ISO 121 515 85% Potassium hydro
xide lentils PA PR 151 628 7.3.1 Liquid silicone defoamer . Sulphuric acid 0.26
N. Dissolve 1.25 g of sulfuric acid 96% PA-ISO in 100 ml of water PAACS. 7.3.2.
Liquid silicone antifoam PR. 7.3.3. Potassium hydroxide solution 0.23 N: Dissolv
e 1.52 g of 85% potassium hydroxide in 100 ml lentils PA PA-ACS Water. 7.3.4. Ac
etone PA-ACS-ISO. 7.3.5. Diethyl Ether stabilized with ~ 6 ppm of BHT PA-ACS-ISO
. 7.4. Procedure. Weigh 1 mg of 1-3 g of sample and add 200 ml of 0.26 N sulfuri
c acid and some drops of liquid silicone antifoam. Bring to a boil and hold for
thirty minutes in a reflux cooling system. After thirty minutes on the filter cr
ucible (7.2.2.) Previously cremated and wash the residue with PA-ACS hot water u
ntil no acid reaction. Quantitatively transfer the residue into a flask adaptabl
e to reflux, add 200 ml of 0.23 N potassium hydroxide and a few drops of antifoa
m. Bring to the boil and boil for thirty minutes. Filter through the crucible an
d wash with hot water PA-ACS until alkaline reaction.€Dehydrate by washing three
times with acetone PA-ACS-ISO using a total volume of 100 ml.
31
Bring the pot to the stove and dried at 130 ° C for two hours. Allow to cool in
desiccator and weigh rapidly. Enter below the crucible in the oven (7.2.3.) And
let burn for three hours at 550 ° C. Allow to cool in desiccator and weigh rapid
ly. 7.5. Calculations. 100 P1 - P2 Crude fiber (%) = P0 ------ Where: P0 = initi
al sample weight. P1 = Weight of the crucible containing the dried sample. P2 =
Weight of the crucible containing the sample calcined. 7.6. Remarks. 7.6.1. Samp
les containing more than 10% fat must be defatted with ethyl ether before analys
is. 7.6.2. To perform the above procedure may be used or semi-automatic systems,
adapting to the equipment specifications. 7.7. References. 7.7.1. Journal Offic
iel des Communautés Européene, number L 83/24, 1973.
121428 131079 211835 131505 131542 172174 171618 131648 181694 181723 131 775
PA Red Mercury II iodide 3-Methyl-1-Butanol PA-ACS Pumice granules Potassium hex
acyanoferrate II QP 3-hydrate PA-ACS-ISO Potassium Iodide PA Luff-Schoorl soluti
on RE Methyl Red Sodium Carbonate 0.1% RE anhydrous PA-ACS-ISO Sodium hydroxide
0.1 mol / l (0,1 N) SV Phenolphthalein indicator Sodium Thiosulphate 0,1 mol / l
(0,1 N) SV Zinc Acetate 2-hydrate PA-ACS
8. SUGARS 8.1. Principle. Elimination of all materials other than reducing sugar
s, using stool from Carrez solutions I, II, upon dissolution of sugars in dilute
ethanol. Elimination of ethanol and valuation before and after the investment b
y the method of Luff-Schoorl. 8.2. Material and apparatus. 8.2.1. Shaker. 8.2.2.
1,000 flasks, 300, 200, 100 and 50 ml. 8.3. Reagents. Glacial Acetic Acid 131 0
08 PA-ACS-ISO 131 018 Citric Acid 1-hydrate PA-ACS-ISO 131 019 Hydrochloric Acid
35% PA-ISO 181023 Hydrochloric Acid 0,1 mol / l (0,1 N) SV 131 058 96% Sulphuri
c Acid PA-ISO PA-ACS Water 131 074 171 096 131 270 RE soluble starch Copper II S
ulphate 5-hydrate PA-ACS-ISO 121 085 Ethanol 96% v / v PA
32
8.3.1. Ethanol 40% (v / v) d = 0.948 to 20 ° C. Dilute Ethanol 96% v / v PA PA-A
CS with water until the concentration indicated. 8.3.2. Carrez solution I. PAACS
Dissolve 24 g of zinc acetate 2-hydrate PA-ACS and 3 ml Glacial Acetic Acid PA-
ACS-ISO and add water-ACS PA up to 100 ml. 8.3.3. Carrez II solution. Dissolve 1
0.6 g PA-ACS Potassium hexacyanoferrate II PA-ACS 3hidrato K4 (FeCN6) 0.3 H2O an
d add 100 ml water PAACS. 8.3.4. Methyl red solution 0.1% RE. 8.3.5. 4N Hydrochl
oric acid. Dilute Hydrochloric Acid 35% PA-ISO with PA-ACS water until the conce
ntration indicated. 8.3.6. Hydrochloric Acid 0.1 mol / l (0,1 N) SV. 8.3.7. Sodi
um hydroxide 0.1 mol / l (0,1 N) SV Phenolphthalein indicator. 8.3.8. Copper Sul
fate Solution. Dissolve 25 g of Copper II Sulfate 5-hydrate PA-ACS-ISO CuSO4.5H2
O, free from iron, PA-ACS in water and dilute to 100 ml. 8.3.9. Citric Acid Solu
tion. Dissolve 50 g of citric acid 1-hydrate PA-ACS-ISO C6H8O7.H2O water in 50 m
l of PA-ACS. 08/03/1910. Sodium Carbonate Solution. Dissolve 143.8 g of anhydrou
s sodium carbonate PA-ACS-ISO in 300 ml of PA-ACS hot water, cool and make up to
300 ml. 03/08/1911. Sodium thiosulfate solution 0.1 mol / l (0,1 N) SV. 08/03/1
912. Starch solution. Add a mixture of 5 g of soluble starch in 30 ml RE PAACS W
ater to 1 liter of water boiling PA-ACS. Let boil for 3 minutes. Allow to cool.
Add 10 mg of PA Red Mercury II iodide as a preservative. 03/08/1913. 6N Sulfuric
Acid. Dilute Sulfuric Acid 96% PA-ISO with PA-ACS water to indicated concentrat
ion. 03/08/1914. Potassium Iodide Solution 30% (w / v). Dissolve Potassium Iodid
e PA-PA-ISO with ACS water to indicated concentration. 08/03/1915. Pumice granul
es QP, washing
M
Hydrochloric Acid 35% PA-ISO and rinse with PA-ACS. 03/08/1916. 3-Methyl-1-Butan
ol PA-ACS. 08/03/1917. Luff-Schoorl RE or prepare as follows: stirring carefully
pour the citric acid solution (8.3.9.) In the solution of sodium carbonate (08.
03.1910.). Stir until the disappearance of the gas release. Then add the copper
sulphate solution (8.3.8.) And up to 1 liter with water PAACS. Let stand twelve
hours and filtered. Check the normality of the reagent thus obtained (Cu 0.1 N;
Na2CO32N). The pH of the solution should be approximately 9.4. 8.4. Procedure. 8
.4.1. Sample preparation. Weigh to the nearest 1 mg, 2.5 g of the sample and pla
ce it in a 250 ml flask. Add 200 ml of ethanol 40% (v / v) and mix for an hour o
n the shaker. Add 5 ml of Carrez I solution and shake for one minute. Add and mi
x in the same time with 5 ml of Carrez II solution.€Make up to 250 ml with 40% e
thanol solution (v / v) (8.3.1.), Mix and filter. 200 ml of filtrate and evapora
te to about half volume to remove most of the ethanol. Transfer the full evapora
tion residue using PA-ACS hot water, a 200 ml flask and cool, then make up with
PA-ACS water and filter if necessary. This solution will be used for the determi
nation of reducing sugars and, after the investment, for the determination of to
tal sugars. 8.4.2. Determination of reducing sugars. Take more than 25 ml of the
solution prepared according to 8.4.1. and containing less than 60 mg of reducin
g sugars expressed as glucose. If necessary, the volume up to 25 ml with water P
A-ACS and to determine the amount of reducing sugars by the Luff-Schoorl. The re
sult will be expressed in per cent of glucose. 8.4.3. Determination of total sug
ars after inversion. Take 50 ml of solution (8.4.1.), Bring to a volumetric flas
k of 100 ml. Add a few drops of Methyl Red 0.1% RE solution and add slowly while
 stirring 15 ml of hydrochloric acid solution 0.1 mol / l (0,1 N) SV and immerse
in a bath of hot water to boil for 30 minutes. Cool to 20 ° C, then add 15 ml o
f sodium hydroxide 0.1 mol / l (0,1 N) SV Phenolphthalein indicator (8.3.7.). Ma
ke up to 100 ml with water and mix PA-ACS. Take a quantity not exceeding 25 ml a
nd containing less than 60 mg of reducing sugars expressed as glucose. If necess
ary, bring the volume to 25 ml with water PA-ACS and to determine the amount of
reducing sugars by LuffSchoorl. The result will be expressed in per cent of gluc
ose. To express sucrose, multiply by 0,95. 8.4.4. Luff-Schoorl rating. Take 25 m
l of Luff-Schoorl reagent (03.08.1917.) And take him to a 300 ml Erlenmeyer flas
k, add 25 ml exactly measured in the clarified sugar solution, add a little QP P
umice granules and heat while stirring. Align a reflux followed the Erlenmeyer f
rom this is done, boil the solution to boiling and boil for ten minutes exactly.
Cool immediately in cold running water for five minutes and proceed to testing.
Add 10 ml of solution of potassium iodide (03.08.1914.) Immediately and careful
ly, 25 ml of 6N sulfuric acid (08.03.1913.). Titrate with sodium thiosulfate sol
ution 0.1 mol / l (0,1 N) SV (08.03.1911.) Until the appearance of yellow color,
then add the starch solution and value terms. Carry out the same assessment of
a mixture containing 25 ml, exactly measured, of Luff-Schoorl, 25 ml of PA-ACS W
ater, 10 ml of solution of potassium iodide (03.08.1914.) And 25 ml of solution
6N Sulfuric Acid (08.03.1913.) without boiling. 8.5. Calculations. Set by Table
I the amount of glucose in mg corresponding to the difference between the two te
sts, according to ml 0.1 N sodium thiosulfate spent on each of the ratings. Expr
ess the result as a percentage of sugars in the sample. 8.6. Remarks. 8.6.1. It
is recommended to add approximately 1 ml of iso-amyl alcohol (regardless of the
volume) before boiling with the reagent LuffSchoorl to avoid foaming. 8.6.2. The
difference between the amount of total sugars after inversion, expressed as glu
cose, and the amount of reducing sugars expressed as glucose also multiplied by
0.95 gives the amount as a percentage of sucrose. 8.6.3. To calculate the amount
of reducing sugars, excluding lactose, can be determined from the following: 8.
6.3.1. A rough estimate, multiply by 0.675 the amount of lactose obtained by det
ermining separately and subtract the result of the amount of reducing sugars. 8.
6.3.2. For precise measurement of reducing sugars, excluding lactose, it is nece
ssary to sample from the same 8.4.1. for the two final determinations. One of th
e analysis is carried out from the solution obtained in 8.4.1. and the other on
part of the solution obtained for assessment of lactose by the method for the de
termination of lactose.
33
Where 8.6.3.1. and 8.6.3.2. the amount of sugars present are determined by the L
uff-Schoorl method, expressed as mg of glucose. The difference between the two v
alues is expressed as a percentage of the sample.
8.7. References. 8.7.1. Journal Officiel des Communautés Européennes, Vol. L 155
/32, 1971.
TABLE 1 To 25 ml of Luff-Schoorl reagent N Na2S203 0.1 ml 1 2 3 4 5 6 7 8 9 10 1
1 12 13 14 15 16 17 18 19 20 21 22 23 Glucose,€invert sugar, fructose C6 H12 06
mg 2.4 4.8 7.2 9.7 12.2 14.7 17.2 19.8 22.4 25.0 27.6 30.3 33.0 35.7 38 , 5 41.3
44.2 47.1 50.0 53.0 56.0 59.1 62.2 2.4 2.4 Variance 2.5 2.5 2.5 2.5 2.6 Februar
y, 6 2.6 2.6 2.7 2.7 2.7 2.8 2.8 2.9 2.9 2.9 3.0 3.0 3.1 3.1 3.6 7.3 mg 11.0 14.
7 18.4 22.1 25.8 29.5 33.2 37.0 40.8 44.6 48.4 52.2 56.0 59.9 63.8 67.7 71, 7 75
.7 79.8 83.9 88.0 Lactose 011 C12 H22 Difference 3.7 3.7 3.7 3.7 3.7 3.7 3.7 3.7
3.8 3.8 3 8 3.8 3.8 3.8 3.9 39 39 4.0 4.0 4.1 4.1 4.1 mg 3.9 7.8 11.7 15.6 19.6
23.5 27 , 5 31.5 35 5 39.5 43.5 47.5 51.6 55.7 59.8 63.9 68.0 72.2 76.5 80.9 85
.4 90.0 94.6 C12 H22 maltose 011 Difference 3.9 3.9 3.9 4.0 3.9 4.0 4.0 4.0 4.0
4.0 4.0 4.1 4.1 4.1 4.1 4.1 4.2 4.3 4.4 4.5 4.6 4.6
9. CHLORIDE 9.1. Principle. The chlorides become soluble in water, defecating if
the solution containing organic matter, subsequent acidifying it with nitric ac
id and precipitation of chloride with silver nitrate. Excess nitrate is titrated
with ammonium thiocyanate solution.
34
9.2. Material and apparatus. 9.2.1. 35-40 shaker r.p.m. 9.3. Reagents. Acetone 1
31 007 PA 131 008-ACS-ISO Glacial Acetic Acid PA-ACS-ISO 131 036 Nitric Acid 60%
PA-ISO
Water 131 074 171 366 PA-ACS iron alum solution saturated ammonium thiocyanate R
E Ammonia 181 144 0.1 mol / l (0,1 N) SV 121 237 132 770 Activated Carbon powder
diethyl ether PA stabilized with ~ 6 ppm of BHT PA-ACS-ISO 181 464 Silver nitra
te 0.1 mol / l (0,1 N) SV 131 505 Potassium hexacyanoferrate II 3-hydrate PA-ACS
131 775 Zinc Acetate 2-hydrate PA-ACS 9.3.1. Ammonium thiocyanate solution 0.1
mol / l (0,1 N) SV. 9.3.2. Silver nitrate solution 0.1 mol / l (0,1 N) SV.
M
9.3.3. Ammonium iron alum saturated solution RE. 9.3.4. Nitric Acid 60% PA-ISO.
9.3.5. Diethyl Ether stabilized with ~ 6 ppm of BHT PA-ACS-ISO. 9.3.6. Acetone P
A-ACS-ISO. 9.3.7. Carrez solution I: dissolve in water PAACS 24 g of zinc acetat
e 2-hydrate PA-ACS and 3 g of glacial Acetic Acid PA-ACS-ISO. Make up to 1000 ml
with water PA-ACS. 9.3.8. Carrez II solution: Dissolve 10.6 g PA-ACS Potassium
hexacyanoferrate II 3hidrato PA-ACS. Up to 100 ml with water PAACS. 9.3.9. Activ
ated Carbon, free from chlorides. Using Activated Carbon powder PA. 9.4. Procedu
re. Weigh 1 mg, 5 g sample and place with 1 g of activated carbon free of chlori
de in a volumetric flask of 500 ml. Add 400 ml of water PA-ACS at 20 ° C and 5 m
l of Carrez I solution, stir and then add 5 ml of Carrez II solution. Stir for 3
0 minutes, make up, mix and filter. Take 25 to 100 ml of filtrate (with chlorine
content less than 150 mg) and place in an Erlenmeyer flask, diluted if necessar
y, up to 50 ml with water PA-ACS. Add 5 ml of Nitric Acid 60% PA-ISO, 20 ml of i
ron ammonium alum RE saturated solution and two drops of ammonia thiocyanate sol
ution 0.1 mol / l (0,1 N) SV, added via a burette filled up the zero line. Add t
hen obtain a burette Silver nitrate solution 0.1 mol / l (0,1 N) SV to an excess
of 5 ml. Add 5 ml of diethyl ether stabilized with ~ 6 ppm of BHT PA-ACS-ISO an
d shake hard to collect the precipitate. Titrate the excess silver nitrate, 0.1
mol / l (0,1 N) SV by ammonia thiocyanate solution 0.1 mol / l (0,1 N) SV until
the shift to dark red lasted for one minute. 9.5. Calculations. The amount of ch
lorine (p) expressed as sodium chloride present in the volume of the solution se
parately for valuation is given by the formula: p = 5.845 (V1 - V2) mg Where: V1
= Volume, in ml of silver nitrate solution added. V2 = Volume in ml Ammonium th
iocyanate solution 0.1 mol / l (0,1 N) SV used in the assessment. Make a blank t
est without the test sample and if you use silver nitrate solution 0.1 mol / l (
0,1 N) SV, subtract this value to volume (V1 - V2). Express the result as a perc
entage of the sample. 9.6. Remarks. 9.6.1. For fat-rich products, scouring previ
ously by ethyl ether. 9.7. References. 9.7.1. Des Communautés européennes Journa
l Officiel No. L 155/23-1971.
10. ZINC 10.1. Principle. Determination of zinc by A.A. after ashing of the samp
le. 10.2. Material and apparatus. 10.2.1. A.A. spectrophotometer 10.2.2. Zinc la
mp. 10.2.3. The use of lead in (11.2.3.) (11.2.4.) (11.2.5.) And (11.2.6.). 10.3
. Reagents. 131 037 Nitric Acid 70% PA-ACS-ISO 131 074 313 193 Water PA-ACS Zinc
standard solution Zn = 1.000 ± 0.002 g / l AA 10.3.1. The use of lead in (11.3.
1.) And (11.3.2.). 10.3.2. Zinc standard solution Zn = 1.000 ± 0.002 g / l AA. 1
0.4. Procedure. 10.4.1. Sample preparation. As in (11.4.1.). 10.4.2. Constructio
n of the calibration curve. Dilute aliquots of the standard solution (10.3.2.) W
ith 1% nitric acid,€to obtain solutions of 0.5, 1.5 and 2 mg / l. 10.4.3. Determ
ination. As for the lead. The reading was performed at 213.5 nm. 10.5. Calculati
ons. Based on the absorbance values obtained, find the concentrations of Zn in t
he sample, taking into account concentration or dilution factor. 10.6. Reference
s. 10.6.1. HEParker: "Atomic Absorption Newsletter" (1963), 13.
35
11. LEAD 11.1. Principle. Determination of lead by A.A. after ashing of the samp
le. 11.2. Material and apparatus. 11.2.1. A.A. spectrophotometer 11.2.2. Lamp le
ad. 11.2.3. Capsule platinum, quartz or similar. 11.2.4. Sand bath or hot plate.
11.2.5. Electric (muffle) with temperature control device. 11.3. Reagents. 131
037 Nitric Acid 70% PA-ACS-ISO 131 074 313 189 Water Lead PA-ACS standard soluti
on Pb = 1.000 ± 0.002 g / l AA 11.3.1. Nitric Acid 70% PA-ACS-ISO (d = 1.413). 1
1.3.2. Nitric Acid 1% PA-ACS water (v / v). Dilute Nitric Acid 70% PA-ACS-ISO PA
-ACS with water until the concentration indicated. 11.3.3. Lead standard solutio
n Pb = 1.000 ± 0.002 g / l AA. 11.4. Procedure. 11.4.1. Sample preparation. Plac
e 10 g of sample in the capsule (11.2.3.), Bring on the hot plate, taking care t
hat the combustion is not too fast so that no loss of solid matter by projection
. Then add 2 ml of 70% Nitric Acid PA-ACS-ISO and char residue in the sand bath
or hot plate. Then insert the capsule into the ring and keep it at 450 ° C until
total mineralization (11.6.1.). Allow to cool. Dissolve the ash with 70% Nitric
Acid PA-ACS-ISO and Water PA-ACS. Bring the solution to a 10 ml flask, washing
the dish with PA-ACS water and add the washings to the mark, then filtered. 11.4
.2. Construction of the calibration curve. Diluting appropriate aliquots of stan
dard solution (11.3.3.) With 1% nitric acid required for its concentration is si
milar to the final dilution of the sample to obtain a curve of concentrations 1,
2 and 3 mg / l. 11.4.3. Determination. Operate according to the specifications
of the appliance, using the air-acetylene flame. Measure the absorbance of the s
ample and standards at 283 nm. If the solution is highly concentrated nitric aci
d diluted with 1%. 11.5. Calculations. Calculate the lead content, expressed as
mg / l by comparison with the corresponding standard curve and taking into accou
nt the dilution factor. 11.6. Remarks. 11.6.1. If the sample is not completely m
ineralized to add a few drops of Nitric Acid 70% PA-ACS-ISO and repeat the proce
ss. 11.7. References. 11.7.1. Official Methods of Analysis of Wines. Ministry of
Agriculture, pp. 134 (I), 1976.
12. MERCURY 12.1. Principle. Determination of mercury by atomic absorption cold
vapor technique after digestion of the sample. 12.2. Material and apparatus. 12.
2.1. Precision balance. 12.2.2. Atomic absorption spectrophotometer. 12.2.3. Mer
cury lamp. 12.2.4. Absorption Chamber quartz windows fitted to the spectrophotom
eter. 12.2.5. Team mercury ion reduction of metallic mercury and drag to the abs
orption chamber including drainage system. 12.2.6. Chart recorder chart speed vo
ltage and variable. 12.2.7. Material Standard laboratory glass washing with nitr
ic acid (1:1) and rinsed with distilled water. 12.2.8. Block digestion temperatu
re. 12.2.9. Digestion tubes for the previous block. 02/12/1910. Condenser tubes
adapted to the digestion tubes. 12.3. Reagents. 131 037 Nitric Acid 70% PA-ACS-I
SO 131 058 96% Sulphuric Acid PA-ISO Water Deionized Water 131 074 PA-ACS Tin II
chloride 10% (Hg free) 141 076 Hydrogen Peroxide 30% w / v (100 vol.) PRS 313 1
86 Mercury standard solution Hg = 1.000 ± 0.002 g / l AA 12.3.1. Sulfuric Acid 9
6% PA-ISO (d = 1.84). 12.3.2. Hydrogen Peroxide 18% w / v. Dilute Hydrogen Perox
ide conveniently 30% w / v (100 vol.) Water PRS with PA-ACS. 12.3.3. Nitric Acid
70% PA-ACS-ISO (d = 1.41). 12.3.4. Tin II chloride 10% (Hg free).
36
M
12.3.5. PA-ACS water. 12.3.6. Mercury standard solution Hg = 1.000 ± 0.002 g / l
AA. 12.3.7. Mercury standard solution of 0.1 mg / l. Is obtained from the above
by successive dilutions with deionized water. Should be prepared as intermediat
e solutions daily. 12.4. Procedure. 12.4.1. Sample Preparation: Place 3 to 5 g o
f sample in a tube digester (12.2.9.) Attaching it to a condensation tube (02.12
.1910.). Add 10 ml Sulfuric Acid 96% PA-ISO in increments of 1 ml (the sample is
charred, but if acid is added slowly so that the temperature of the solution to
 remain low, and take care that no forming masses of coal,€mercury remains in so
lution). Add 10 ml of Hydrogen Peroxide 18% w / v (12.3.2.) Increments of 1 ml.
Allow to react before adding the next increment. Add 10 ml of Nitric Acid 70% PA
-ACS-ISO in increments of 1 ml. Wash with water condensers and remove PA-ACS. 12
.4.2. Digestion of the sample digestion Place tubes in the heating block and hea
t at 100 ° C. Maintain this temperature for 6 minutes, then increase to 200 ° C
at 4 ° C / minute. Remove the tubes from the block and let cool. Transfer the so
lutions to 100 ml flasks and dilute with water PA-ACS. 12.4.3. Determination: th
e sample is analyzed by cold vapor AA according to the instructions of each devi
ce, using 10% Tin II chloride (Hg free) as a reducing agent (12.3.4.) being the
measurement wavelength 254 nm. 12.4.4. Construction of the calibration curve: Ob
tained abscissa representing mercury content of the standards prepared with aliq
uots of 0, 0.5, 1.0, 2.0, 5.0 and 10 ml of standard solution of 0.1 mg / l to co
ntain 0-1 mg of mercury and ordered to the height of the corresponding absorptio
n maxima. These patterns have undergone the same procedure as samples. 12.5. Cal
culations. Calculate the mercury content by referring to the standard curve prev
iously obtained under identical operating conditions. P = weight in grams of the
sample. 12.6. References. 12.6.1. Munns and Holland. JAOAC 60 833-837, 1977. 12
.6.2. Marts and Blahc. JAOAC vol. 66, No. 6 1983. 12.6.3. AOAC Official Methods
of Analysis, 1980.
13. COPPER 13.1 Principle. Determination of copper by A.A. after ashing of the s
ample. 13.2. Material and apparatus. 13.2.1. A.A. spectrophotometer 13.2.2. Bras
s lamp. 13.2.3. The lead used in (11.2.3.) (11.2.4.) And (11.2.5.). 13.3. Reagen
ts 131 037 Nitric Acid 70% PA-ACS-ISO 131 074 313 178 Water PA-ACS Copper Cu sta
ndard solution = 1.000 ± 0.002 g / l AA 13.3.1. The lead used in (11.3.1.) And (
11.3.2.). 13.3.2. Copper standard solution Cu = 1.000 ± 0.002 g / l AA. 13.4. Pr
ocedure. 13.4.1. Sample preparation. As in (11.4.1.). 13.4.2. Construction of th
e calibration curve. Dilute aliquot of standard solution (13.3.2.) With 1% nitri
c acid to obtain solutions containing from 1-5 mg Cu / l. 13.4.3. Determination.
As for the lead. Measured at 324.7 nm. 13.5 Calculations. From the absorbance v
alues obtained for the sample, found by the standard curve concentrations of cop
per in the sample. 13.6 References. 13.6.1. H. E. Parker: "Atomic Absorption New
sletter (1963), 13." 13.6.2 F. Rousselet: "Spectrophotometrie absorption atomiqu
e pour Boudin" Ed Paris (1968), pp. 59-144.
L Hg mg / Kg = - P, where: L = A reading from the graph expressed in micrograms.
37
14. ARSENIC 14.1. Principle. The sample is subjected to acid digestion with a mi
xture of nitric and sulfuric acid. The determination of arsenic was done by atom
ic absorption spectrophotometry with hydride generator. 14.2. Material and appar
atus. 14.2.1. Analytical balance accurate to 0.1 mg. 14.2.2. Kjeldahl flasks of
250 ml. 14.2.3. Atomic absorption spectrophotometer equipped with hydride genera
tor system. 14.2.4. Electrodeless discharge lamp. 14.2.5. Power supply for disch
arge lamp without electrodes. 14.2.6. Graphic recording. 14.3. Reagents. They ar
e only used pure reagents and distilled water for analysis. 131 020 Hydrochloric
Acid 37% PA-ACS-ISO 131 669 Ethylenediaminetetraacetic acid disodium salt 2-hyd
rate PA-ACS-ISO 131 037 Nitric Acid 70% PA-ACS-ISO 131 058 96% Sulphuric Acid IS
O PA-PA-ACS 131 074 313 171 Water Arsenic standard solution As = 1.000 ± 0.002 g
/ l AA 121 515 85% Potassium Hydroxide Sodium borohydride lentils PA PA 123 314
131 687 Sodium hydroxide lentils PA-ACS-ISO 14.3.1. Hydrochloric Acid 37% PA-AC
S-ISO (d = 1.19 g / ml). 14.3.2. Hydrochloric acid solution 32% v / v. Dissolve
32 ml of 37% Hydrochloric Acid with Water-ISO PAACS PA-ACS to a volume of 100 ml
. 14.3.3. Hydrochloric acid solution 1.5% v / v. Dissolve 15 ml of 37% Hydrochlo
ric Acid with Water-ISO PAACS PA-ACS to a volume of 1000 ml. 14.3.4. Nitric Acid
65% (d = 1.40). Dilute Nitric Acid 70% PA-ACS-ISO with PA-ACS water until the c
oncentration indicated. 14.3.5. Sulfuric Acid 96% PA-ISO (d = 1.84). 14.3.6. Sol
ution of Sodium Hydroxide 1%. Weigh 1 g of sodium hydroxide lentils PA-ACS-ISO a
nd dissolved with PA-ACS water to a volume of 100 ml. 14.3.7. Dissolution of sod
ium borohydride to 3%. Weigh 3 g of sodium borohydride PA and dissolve to 100 ml
with 1% sodium hydroxide. 14.3.8. Dissolution of EDTA disodium salt 2-hydrate a
t 1%.€Weigh 1 g EDTA disodium salt 2-hydrate PA-ACS-ISO and dissolved to 100 ml
with water PA-ACS.
14.3.9. Potassium Hydroxide Solution 20%. Weigh 20 g 85% Potassium hydroxide len
tils with water and dissolved PA PA-ACS to a volume of 100 ml. 03/14/1910. Sulfu
ric acid solution 20% (v / v). Dilute Sulfuric Acid 20 ml of 96% PA-ISO (14.3.5.
) PA-ACS with water to a volume of 100 ml. 03/14/1911. Sulfuric acid solution 1%
(v / v). Dilute 1 ml of Sulfuric Acid 96% PA-ISO with PA-ACS water to a volume
of 100 ml. 03/14/1912. Arsenic standard solution As = 1,000 ± 0,002 g / l AA. 03
/14/1913. Arsenic standard solution of concentration 10 mg / l. Pipette 1 ml of
standard solution of arsenic (03.14.1912.) In a 100 ml flask. Dilute to the mark
with water PA-ACS. 14/03/1914. Arsenic standard solution of concentration 0.1 m
g / l. Pipette 1 ml of the solution of arsenic (14.03.1913.) In a 100 ml flask.
Dilute to the mark with water PA-ACS. 14.4. Procedure. 14.4.1. Sample preparatio
n .- In a Kjeldahl flask, 250 ml of 2 g of sample with 20 ml of nitric acid and
5 ml 65% Sulphuric Acid 96% PA-ISO. Boil until a volume of 5 ml. Cool and dissol
ve PA-ACS water in a flask of 50 ml of the resulting solution. 14.4.2. Preparati
on of the target and work patterns. In a Kjeldahl flask, introduce 5 ml of the s
olution of arsenic (03.14.1914.) And subject to the same treatment as the sample
. 1 ml of solution containing 10 ng of arsenic. Prepare a blank with all reagent
s used following the treatment of the sample. 14.4.3. Terms of espectrofotómetro
.Encender the power supply discharge lamps without electrodes with sufficient ti
me to stabilize the energy of the lamp. Turn on the spectrophotometer, set the w
avelength of 193.7 nm, placing the grid in accordance with the conditions of the
device. Turn the hydride generator by placing the cell temperature to 900 ° C,
waiting until it reaches that temperature. In conformity with the conditions of
hydride generation as specified by the appliance. Adjust the flow of argon accor
ding to the characteristics of the device. Turn on the recorder. 14.4.4. Determi
nation .- Any determination of the concentration of arsenic was performed by the
method of standard addition, by duplicate measures in the spectrophotometer und
er the conditions specified in (14.4.3.) Adding to the reaction flask 3 ml of so
lution (14.3.8.) using the solution as a reducing agent (14.3.7.) are used as in
ternal standards 10, 20 and 50 ng Aires
38
M
Wash the flasks before and after each use with 1.5% hydrochloric acid (14.3.3.).
In constructing the graph of addition is to discount the value of absorbance of
the blank obtained in the same conditions as before, but adding 3 ml of blank s
olution. Under these conditions the detection limit of the technique is 5 ng.
39
Pasta
40
M
METHODS OF ANALYSIS (B.O.E. 08/09/1987) 10. DEGREE OF ACIDITY 10.1. Principle. T
he acidity of the alcoholic extract of pasta is determined by titration and expr
essed in ml of 1N NaOH. 10.2. Material and apparatus. 10.2.1. Laboratory mill, w
ithout heating the sample to be able to obtain particles less than 550 microns.
10.2.2. Rapid filtration filter. 10.3. Reagents. PA-ACS Water 131 074 121 085 Et
hanol 96% v / v PA Phenolphthalein solution 1% 171 327 182 296 RE Sodium Hydroxi
de 0,025 mol / l (0,025 N) SV 10.3.1. 95 ° ethanol, peroxide-free. 10.3.2. Ethan
ol 50 °. Mix 100 ml of ethanol 95 ° with 96 ml of water PA-ACS. 10.3.3. Sodium h
ydroxide 0.025 mol / l (0,025 N) SV or lentils prepared by dissolving sodium hyd
roxide in water-ISO PAACS PA-ACS, to the concentration indicated. 10.3.4. Phenol
phthalein solution 1% RE. 10.4. Procedure. Grind the sample to be analyzed thoro
ughly so that it passes through a mesh sieve of 500 microns. Weigh one milligram
, 4 g of product, transferring to a 500 ml Erlenmeyer flask with ground stopper,
and add 100 ml of ethanol 50 ° previously neutralized to phenolphthalein with N
aOH 0.02 N. Shake vigorously and allow contact with the alcohol solution for thr
ee hours, stirring periodically. After a period of three hours, filtered through
the filter 10.2.2. Take 50 ml of the filtrate and titrate with 0.02 N NaOH, usi
ng as three drops of phenolphthalein indicator solution 1% RE. 10.5. Expression
of results. It defines the degree of acidity (G) as the number of ml 1N sodium h
ydroxide to neutralize the acidity of 100 g of dry product. G = V x 100 ---- 100
- H where: V = Volume in ml of 0.02 N NaOH used for neutralization. H = Percent
age of moisture in the sample.€Express the result to one decimal place.
41
Cookies
42
M
METHODS OF ANALYSIS (B.O.E. 11/24/1987) 10. REMOVAL OF GREASE FOR IDENTIFICATION
10.1. Principle. Extraction of fat with petroleum ether by continuous extractio
n apparatus. 10.2. Material and apparatus. 10.2.1. Soxhlet type extractor. 10.2.
2. Extraction cartridges. 10.2.3. Flasks of 100-150 ml adaptable to the extracto
r. 10.2.4. Battery removal. 10.3. Reagents. 131 315 Petroleum Ether 40-60 ° C PA
-ISO 10.3.1. Petroleum Ether 40-60 ° C PA-ISO. 10.4. Procedure. Take 5 to 10 g o
f sample, prepared by method 1, and perform the extraction with petroleum ether
40-60 ° C PA-ISO, the continuous extraction apparatus (10.2.1.) At a temperature
between 4060 ° C . 10.5. Remarks. 10.5.1. In the case of fat needed for the det
ermination of components that can be altered to 60 ° C, can be made cold extract
ion using ethyl ether or chloroform-ethanol (1:1).
43