Astm E534 - 08
Astm E534 - 08
Astm E534 - 08
8.6 Slowly add the salt sample to the high-speed blender B = mass of sample, g.
and blend for 5 min.
8.7 Test for water insolubles as described in Sections 17-24. 15. Report
8.8 Save filtrate from water insolubles test and dilute in a 15.1 Report the moisture content to the nearest 0.001 %.
volumetric flask to 1 L with water as a stock solution for
subsequent analyses. 16. Precision and Bias
16.1 The following criteria should be used in judging the
9. Evaporated and Purified Salt Stock Solutions acceptability of results (Note 1):
9.1 Mix and split the sample to 100 g for evaporated salt, or 16.1.1 Repeatability (Single Analyst)—The standard devia-
200 g for purified evaporated salt. tion for a single determination has been estimated to be the
9.2 Transfer to a 1-L volumetric flask. percent absolute values shown in Table 1 at the indicated
9.3 Add 800 mL of water and allow the salt to dissolve. degrees of freedom. The 95 % limit for the difference between
9.4 Add 2 mL of concentrated HCl to dissolve any water two such runs is the percent absolute values in Table 1.
insoluble calcium salts, particularly calcium carbonate. 16.1.2 Laboratory precision (Within-Laboratory, Between-
9.5 Dilute to volume with water and use as a stock solution Days Variability)—The standard deviation of results (each the
for subsequent analyses. average of duplicates), obtained by the same analyst on
different days, has been estimated to be the percent absolute
MOISTURE values shown in Table 1 at the indicated degrees of freedom.
The 95 % limit for the difference between two such averages is
10. Scope
the percent absolute values in Table 1.
10.1 This test method determines free moisture in the salt 16.1.3 Reproducibility (Multilaboratory)—The standard de-
over a concentration range from 0.00 to 0.04 %. It does not viation of results (each the average of duplicates), obtained by
determine occluded moisture trapped within the salt crystals. analysts in different laboratories, has been estimated to be
The procedure is based on weight loss after a sample is heated percent absolute values shown in Table 1. The 95 % limit for
to volatize moisture. the difference between two such averages is the percent
absolute values in Table 1.
11. Apparatus
11.1 Analytical Balance. NOTE 1—The preceding precision statements are based on an interlabo-
ratory study performed around 1975 on five samples of sodium chloride
11.2 Desiccator. containing covering the ranges of moisture in Table 1. One analyst in each
11.3 Oven. of ten laboratories performed duplicate determinations and repeated them
on a second day.4 Practice E 180 was used in developing these precision
12. Procedure, Rock and Solar Salt estimates.
12.1 Weigh 100 g of salt to the nearest 0.05 g into a 16.2 Bias—The bias of this test method has not been
previously dried and tared moisture dish. determined due to the unavailability of suitable reference
12.2 Dry at 110°C for 2 h. materials.
12.3 Cool in a desiccator and weigh.
WATER INSOLUBLES
13. Procedure, Evaporated and Purified Evaporated Salt
13.1 Weigh 20 g of salt to the nearest 0.001 g into a 17. Scope
previously dried and weighed glass weighing bottle and cover. 17.1 This gravimetric method determines only the amount
13.2 Dry at 110°C for 2 h. of insolubles present in sodium chloride which will not
13.3 Cool in a desiccator, replace cover, and weigh. dissolve in water.
where: 4
Supporting data have been filed at ASTM International Headquarters and may
A = loss of mass on drying, g, and be obtained by requesting Research Report RR: E15–1052.
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26. Apparatus
26.1 Magnetic Stirrer with Stirring Bar. 28. Procedure
28.1 Using Table 3 as a guide, pipet two aliquots of stock
27. Reagents solution into 400-mL beakers to give a titer between 2 and 10
27.1 Eriochrome Black T Indicator Solution, Hydroxy mL of standard EDTA solution. One aliquot is used to
Naphthol Blue, or its equivalent. determine total calcium and magnesium and the other for
27.2 Murexide (Ammonium Purpurate) Indicator Solution, calcium.
or its equivalent. 28.2 Dilute to 200 mL with water, if necessary, and place on
27.3 EDTA Standard Solution (1 mL = 0.400 mg calcium)— magnetic stirrer.
Dissolve 4.0 g of disodium dihydrogen ethylene diaminetet- 28.3 Total Calcium and Magnesium:
raacetate (EDTA) in 1 L of water. Standardize this solution 28.3.1 Add 5 mL of buffer solution, 1 mL of KCN solution,
against a standard calcium solution prepared by dissolving and a sufficient amount of Eriochrome Black T Indicator
1.000 g of CaCO3 and 2 mL of HCl in water and diluting to 1 Solution or its equivalent.
L with water in a volumetric flask. Obtain an exact factor for 28.3.2 Titrate with standard EDTA solution to a true blue
the EDTA solution. This factor is equal to the milligrams of color.
calcium equivalent to 1.00 mL of EDTA solution. See Practice 28.3.3 Record the millilitres used as Titration 1 (T1).
E 200. 28.4 Calcium Only:
W 28.4.1 Add 2 mL of KOH solution, 1 mL of KCN solution
factor 5 V (3) to the other aliquot in 28.1 and 28.2, and stir for about 2 min
to precipitate magnesium.
where: 28.4.2 Add a sufficient amount of murexide solution or an
W = calcium in aliquot, mg, and equivalent calcium indicator solution.
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V = EDTA solution required for titration, mL. 28.4.3 Titrate with standard EDTA solution to a true blue
27.4 Ammonium Chloride–Ammonium Hydroxide color.
Solution—Add 67.5 g of ammonium chloride (NH 4Cl) to 570 28.4.4 Record the millilitres used as Titration 2 (T2).
mL of ammonium hydroxide (NH4OH) contained in a 1-L
volumetric flask. Reserve this solution for use as described in 29. Calculation
27.6 and 27.7. 29.1 Calculate the mass percent of calcium as follows:
27.5 Potassium Cyanide Solution (50 g/L)—Dissolve 50 g
of potassium cyanide (KCN) in water and dilute to 1 L with ~T2! ~factor! ~0.1!
Ca, % mass ~m/m! 5 S (4)
water. Store in a borosilicate glass bottle. (Warning—
Potassium cyanide is extremely poisonous.) where:
27.6 Magnesium Sulfate Solution (2.5 g/L)—Dissolve 2.5 g T2 = EDTA used to titrate calcium only, mL.
of MgSO4·7H2O in water and dilute to volume with water in a S = mass of salt in aliquot, g.
1-L volumetric flask. Determine the volume of EDTA solution 29.1.1 See 27.3 for factor.
equivalent to 50 mL of MgSO4 solution as follows: Pipet 50 29.2 Calculate the mass percent of magnesium as follows:
mL of MgSO4 solution into a 400-mL beaker. Add 200 mL of
~T1 2 T2! ~factor! ~0.6064! ~0.1!
water and 2 mL of NH4Cl:NH4OH solution (27.4). Add 1 mL Mg, % mass ~m/m!5 S (5)
of KCN solution and a sufficient amount of Eriochrome Black
T Indicator solution or its equivalent. Titrate the solution with where:
EDTA solution while stirring with a magnetic stirrer to the true T1 = EDTA used to titrate total calcium and magnesium,
blue end point. This gives the volume of EDTA solution S = mass of salt in aliquot, g.
equivalent to 50.0 mL of MgSO4 solution.
27.7 Buffer Solution—Pipet 50 mL of MgSO4 solution into 30. Report
the volumetric flask containing the remaining NH4Cl·NH4OH 30.1 Report the percentage of calcium to the nearest
solution (27.4). Add the exact volume of EDTA solution 0.001 %. Report the percentage of magnesium to the nearest
equivalent to 50 mL of the MgSO4 solution. Dilute to 1 L with 0.001 %.
water. Store the solution in a polyethylene bottle.
27.8 Potassium Hydroxide Solution (600 g/L)—Dissolve 31. Precision and Bias
150 g of potassium hydroxide (KOH) in 250 mL of water. Cool 31.1 The following criteria should be used in judging the
and store in a polyethylene bottle. acceptability of calcium results (Note 3):
31.1.1 Repeatability (Single Analyst)—The coefficient of 31.2.4 Bias—The bias of this test method has not been
variation for a single determination has been estimated to be determined due to the unavailability of suitable reference
3.56 % relative at 100 df. The 95 % limit for the difference materials.
between two such runs is 10 % relative.
31.1.2 Laboratory Precision (Within-Laboratory, Between- SULFATE
Days Variability)—The coefficient of variation of results (each
the average of duplicates), obtained by the same analyst on 32. Scope
different days, has been estimated to be 6.34 % relative at 40 32.1 This test method covers the gravimetric determination
df. The 95 % limit for the difference between two such of the sulfate content of sodium chloride.
averages is 18 % relative.
31.1.3 Reproducibility (Multilaboratory)—The coefficient 33. Apparatus
of variation of results (each the average of duplicates), ob-
tained by analysts in different laboratories, has been estimated 33.1 Gooch Asbestos Slurry.
to be 9.82 % relative at 7 df. The 95 % limit for the difference 33.2 Gooch Filtering Crucible and Holder.
between two such averages is 28 % relative. 33.3 Muffle Furnace.
33.4 Oven.
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Subcommittee E15.02 has identified the location of selected changes to this standard since the last issue
(E 534-98(2003)) that may impact the use of this standard.
(1) Updated units of measure to comply with the International units are to be considered standard.
System of Units (SI). (3) Added Summary of Changes section.
(2) Added numbered paragraph in Scope stating that the SI
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