Prelegere 2 Control calitate 15 martie 2019

1.Benzene
Quality Specifications

The ASTM has specified standards and test methods for benzene and related
aromatic compounds. Likewise, specifications have been developed and used
in other countries. As examples, the American National Standards have been
used. The DIN Standards are used in Germany, and those of the Institute of
Petroleum in England. The Technical Committee of ISO has standardized
many of the specifications and test methods. Many of the ASTM methods
have an Institute of Petroleum designation also.
The ASTM specifications for different grades of benzene are shown in Table
(22). Test methods developed by ASTM are used in determining the specific
properties of benzene:
1) Sampling: method D-270 for petroleum and petroleum products
2) ASTM D-891: specific gravity
3) ASTM D-1209: color
4) ASTM D-850: distillation
5) ASTM D-852: freezing point
6) ASTM D-848: wash color
7) ASTM D-847: acidity
8) ASTM D-849: copper corrosion
9) ASTM D-853: sulfur compounds
10) ASTM D-1685: thiophene
11) ASTM D-2360: nonaromatics

Similar specifications and tests have been developed for related aromatic
compounds as well as for reagent grades of other materials; e.g., ASTM
methods D-362–75 and D-841–71 describe standard specifications for
industrial and for nitration-grade toluene.
The concentration of nonaromatics permitted in different grades of benzene
is limited and in most cases must not exceed 0.15%. For the 5.5 °C freezing
point grade the maximum allowable is 0.01%. The amount of paraffinic and
naphthenic materials in the finished benzene is reflected in the boiling range
and freezing point of the benzene.
The tests outlined by the ASTM methods and similar tests in different
countries characterize benzene purity and whether or not the desired
specifications are met. Gas chromatography is an important and efficient
method for determining the presence of impurities in benzene and also the
amount of benzene in different potential charge stocks available for the
production of benzene.
Specifications for different grades of benzene

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Specification Industrial grade Refined benzene-535 Refined benzene-485

(ASTM D836–71) (ASTM D2359–69) (nitration grade)
(ASTM D835–71)
Appearance clear, water white
Specific gravity (15.56/15.56 °C) 0.875–0.886 0.882–0.886 0.882–0.886
Color not darker than 20 max. 20 max. 20 max.
Distillation range at 101.3 kPa not more than 2.0 °C not more than 1.0 °C not more than 1.0 °C
Solidification point 5.35 °C min. (dry basis) 4.85 °C min. (dry basis)
Acid wash color not darker than no. 3 no. 1 max. no. 2 max.
Acidity no free acid nil no evidence of acidity
H2S, SO2 free

Thiophene 1 ppm
Sulfur compounds free of H2S and SO2 free of H2S and SO2

Copper corrosion copper strip strip shall not show irridescence nor a gray or black deposit or discoloration
Nonaromatics 0.15% max.
Carbon disulfide if needed use ASTM D2324
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2.Specifications of Butadiene

The butadiene specification necessary to meet the market requirements today

is listed in Table (8). The purity requirements have been intensified because
the Ziegler-type catalysts employed in the stereospecific synthesis of rubbers
are sensitive to, for example, allenes and acetylenes. The purity requirements
are less stringent for butadiene used in emulsion polymerization, such as in
the synthesis of styrene–butadiene rubber and latex [85]. However, a high
degree of purity is generally required today for butadiene in world trade.

Typical specifications of butadiene

Compound Specification Test method
1,3-Butadiene  99.6% ASTM-D 2593-86
Propyne max. 5 ppm ASTM-D 2593-86
Propadiene max. 2 ppm ASTM-D 2593-86
Vinylacetylene max. 5 ppm ASTM-D 2593-86
Ethylacetylene max. 2 ppm ASTM-D 2593-86
 Acetylenes (calculated max. 20 ppm ASTM-D 1020-76
as vinylacetylene)
Dimerics max. 250 ISO 7381
ppm*
1,2-Butadiene max. 30 ppm ASTM-D 2593-86
Carbonyls max. 25 ppm ASTM-D 4423-91
(calculated as CH3CHO)

Sulfur max. 1 ppm ASTM-D 3246-76

Peroxides max. 1 ppm ASTM-D 1022-76
(calculated as H2O2)

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Methanol max. 10 ppm ISO 8174

H2O max. 5 ppm ISO 6191

Residue max. 10 ppm ASTM-D 2593-86

Inhibitor TBC** 75–125 ppm ASTM-D 2593-86
Oxygen in the gas phase max. 0.1 vol% ASTM-D 2593-86
* Maximum set by battery producers;
** TBC=tert-butylpyrocatechol

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3.Butenes
Quality Specifications

Due to different production processes and applications, no standard quality

specifications for the butenes are available. The two isomers which have
become commodities as high purity products show in general a purity greater
than 99 wt%. Table (5) illustrates the typical isobutene and 1-butene
composition as obtained through the Hüls processes.

Isobutene and 1-butene composition (in wt%) in high-purity

commercial products (Hüls)
Component Isobutene 1-Butene
Isobutene 99.98 0.15
1-Butene 0.005 99.70
2-Butenes 0.01 < 0.01
Butanes 0.005 0.15
1,3-Butadiene < 0.001 < 0.001
tert-Butanol < 0.0005 < 0.0001
Water < 0.003 < 0.001
Sulfur < 0.0001 < 0.0001

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4.Cyclohexane
Quality Specifications and Tests

The typical purity specification for cyclohexane is 99.9 wt% min. Impurities
are unconverted benzene, aliphatic hydrocarbons in the benzene feed to the
hydrogenation unit, methylcyclopentane formed by isomerization of
cyclohexane, and methylcyclohexane formed by hydrogenation of the small
amount of toluene in benzene. Freezing point, punctul de congelare relative
density, and a distillation range of 1 °C, with 80.7 °C in the range, are
generally specified. A sulfur level of less than 1 mg/kg as measured by ASTM
method D-3120 is also specified. In addition, specifications of phenol,
chloride, and basic nitrogen content exist, but they are of little importance
because the levels of these in product cyclohexane are generally less than 0.1
mg/kg. Although these specifications, with the appropriate ASTM test method,
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are used in contractual agreements between cyclohexane producers and their

customers, gas chromatography is generally employed for quality control in
manufacturing because of its precision and reproducibility.
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5.Ethylbenzene
Quality Specifications

The product specification on ethylbenzene is set to provide a satisfactory

feedstock to the associated styrene unit. Objectionable impurities in the
ethylbenzene can be grouped into two categories: those that are detrimental
to the operation of the styrene unit and those that affect the purity of the
styrene product. Impurities in product ethylbenzene that pose an operating
problem in the conventional dehydrogenative styrene process are
1) Halides, which deactivate the dehydrogenation catalyst and contribute
to downstream equipment corrosion. Usually these are chlorides originating
from an AlCl3 alkylation section or fluorides from an Alkar unit.
2) Diethylbenzenes, which are dehydrogenated to divinylbenzenes in the
styrene reactor section. The divinylbenzenes form insoluble cross-linked
polymers in the downstream process equipment. A limit of less than 10 ppm
of diethylbenzenes in the ethylbenzene product is usually imposed.
Ethylbenzene contaminants that can affect styrene purity are components
having a boiling range between ethylbenzene and styrene. These include
xylenes, propylbenzenes, and ethyltoluenes. The levels of cumene, n-
propylbenzene, ethyltoluenes, and xylenes in the ethylbenzene is controlled
to meet the required styrene purity specification.
A typical sales specification for a United States manufacturer is a follows:
Purity 99.5 wt% min.
Benzene 0.05–0.3 wt%
Toluene 0.1–0.3 wt%
Xylenes 0.2 wt% max.
Nonaromatics 0.05 wt% max.
Propylbenzenes 0.02 wt% max.
Diethylbenzenes 10 mg/kg max.
–
Total chlorides as Cl 1–3 mg/kg
max.
Total organic sulfur 4 mg/kg max.
Relative density at 15 °C 0.869–0.872
APHA Color 15 max.

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APHA color, also referred to as the Hazen scale, and more appropriately as the Platinum
Cobalt(Pt/Co) scale,[1] is a color standard named for the American Public Health Association
and defined by ASTM D1209. It was originally intended to describe the color of waste water,
but its usage has expanded to include other industrial applications. APHA color is a color
scale sometimes referred to as a "yellowness index" that is used to assess the quality of
liquids that are clear to yellowish in color.
It is similar to the Hazen color test, to which it is sometimes incorrectly referred. The Hazen
color test uses a Pt/Co solution and was developed for water treatment facilities where the
Color of water could be used as a measure of concentration of dissolved and particulate
material. Slight discoloration is measured in Hazen units (HU).[2] Impurities can be deeply
colored as well, for instance dissolved organic compounds called tannins can result in dark
brown colors.
In the chemical, pharmaceutical and plastics industries, APHA/Pt-Co/Hazen is used to
differentiate trace amounts of yellowness in near colorless or low chroma liquid samples.
APHA/Pt-Co/Hazen has a range from 0 (distilled water) to 500 (pale yellow) and is used to
differentiate small amounts of yellowness in near “water-white” liquids.
The Gardner Color is used to differentiate higher chroma yellow samples that also vary in
lightness and hue. The Gardner Color Scale was originally based on liquid chloroplatinate
standards before the defintion of the Gardner Color Scale was re-set in 1958 to a set of 18
color filters designed to match the color of the original liquid standards.
The Gardner Color scale ranges from 0 (distilled water) to 1 (light yellow), then continues to
a dark, murky 18. Over the 0 to 18 range, there is an increase in yellowness, decrease in
lightness and change in hue from a red yellow to green yellow. Most applications range
from 0 to 8 in Gardner Color.
The point of crossover between APHA/Pt-Co/Hazen and Gardner color is at the top end of the
APHA/Pt-Co/Hazen scale and the corresponding low-end of the Gardner Color scale. An
APHA/Pt-Co/Hazen 500 color standard is considered to be just under a Gardner 2.
There are some applications where evaluation of process color quality can be done with
a combination of APHA and Gardner Color. A material may begin as a highly yellow liquid
that measures a mid-level Gardner Color. With refining, the color quality improves and results
in a less yellow Gardner 2 or 1. As the refining process continues, the products are more water
white. APHA can be used to measure the product as it is further refined to desired color end
point near water. The final measured result may also be used to document a sales quality
specification of “APHA Color less than 30”.
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6.Ethylene
Quality Specifications

Ethylene quality worldwide is matched to customer requirements; no single

chemical-grade ethylene exists. However, ethylene content normally exceeds
99.9 wt%. The reason for variation in ethylene specifications is due to the
use of ethylene in downstream processes that differ in sensitivity to
impurities in ethylene, due to different catalyst systems being used. In
general, the trend is towards lower impurity contents as more active catalyst
systems are developed. The largest application for ethylene is polymerization
to HDPE, LDPE, and LLDPE. For these processes new catalyst systems have

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been developed, including the metallocene catalysts, which are more

sensitive than other catalysts. Table (11) lists typical ethylene specifications
for various polymerization processes.
Sulfur, oxygen, acetylene, hydrogen, carbon monoxide and carbon dioxide
are the most troublesome and carefully controlled impurities, especially
when ethylene from multiple sources is mixed in transportation.
Polietilena Polietilena este un polimer termoplastic cu o structură cristalină variabilă
și o gamă extrem de largă de aplicații practice în diferite domenii de activitate. De altfel,
polietilena este materialul plastic produs în cea mai mare cantitate la nivel mondial, cu zeci
de milioane de tone produse anual.
Procesul său de producție comercială, a fost implementat de către Karl Ziegler și Giulio
Natta în anii 50 ai secolului trecut. De atunci, polietilena a devenit treptat cel mai de succes
produs sintetic cu varii aplicații în funcție de tipul de material produs.
Da, polietilena se prezintă în mai multe forme de compoziție, fiecare având destinațiile sale
precise. Principalele tipuri de polietilena sunt următoarele:
Polietilena de joasă densitate (LDPE/PEJD)
Se prezintă sub forma unui material foarte flexibil, proprietate care îl face ușor de procesat și
extrem de maleabil, una dintre aplicațiile cele mai cunoscute fiind plasele pentru
cumpărături. Polietilena de joasă densitate se mai remarcă printr-un cost scăzut de
producție, rezistență chimică foarte mare și proprietăți excelente de izolare electrică.
Polietilena liniară de joasă densitate (LLDPE/PELJD)
Este similară polietilenei de joasă densitate. Diferența este dată de faptul că proprietățile
acestui tip de material plastic pot fi alterate prin schimbarea elementelor chimice din
formulă. În același timp, procesul de producție al polietilenei liniare presupune un consum
mai scăzut de energie. Se folosește în industria alimentară, agricultură, construcții și
fabricarea mobilierului.
Polietilena de mare densitate (HDPE/PEID)
Se deosebește de celelalte tipuri de polietilenă prezentate până acum prin procesul său de
producție, de presiune joasă, care îi conferă un punct de topire mai înalt și o densitate mai
mare. Materialul rezultat este dur, ușor de turnat cu rezistență înaltă la impact. Este utilizat
în mod frecvent în industrie pentru fabricarea cutiilor de lapte, a cutiilor pentru detergenți
sau a containerelor pentru gunoiul menajer.
Polietilena de masă moleculară ridicată (UHMW)
Reprezintă o versiune extrem de densă a polietilenei cu o masă moleculară considerabil mai
mare decât ce a HDPE. Firele de UHMW sunt de multe ori mai rezistente decât oțelul, motiv
pentru care una dintre aplicațiile acestui tip de material plastic sunt vestele anti-glonț și
echipamentele de înaltă performanță.
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